A nickel-based oxide dispersion-strengthened alloy material and its preparation method

Abstract

This invention discloses a nickel-based oxide dispersion-strengthened alloy material and its preparation method. The alloy material is prepared by mixing two nickel-based alloy powders with different melting points. The specific compositions are as follows: the high-melting-point alloy powder consists of 74.1–77.1 wt.% nickel, 20 wt.% chromium, 0.5–2 wt.% titanium, 0.5–2 wt.% niobium, 1 wt.% iron, 0.3 wt.% aluminum, and 0.6 wt.% nano-yttrium oxide; the low-melting-point alloy powder consists of 77.6–79.6 wt.% nickel, 20 wt.% chromium, 6–8 wt.% zirconium, 2 wt.% boron, 1 wt.% iron, 0.5 wt.% titanium, 0.3 wt.% aluminum, and 0.6 wt.% nano-yttrium oxide. The low-melting-point alloy powder accounts for 1–3% of the total mass of the mixed powder. This invention achieves isothermal solidification by using spark plasma sintering of alloy powders with high and low melting points. This is achieved by utilizing the diffusion of demelting elements from the low-melting-point alloy to the high-melting-point alloy during melting. This reduces the sintering temperature and shortens the holding time of the oxide dispersion-strengthened alloy, avoiding the failure of dispersion strengthening caused by oxide agglomeration at high temperatures. This improves the mechanical properties of the alloy, giving it higher strength and hardness.

Description

Technical Field

[0001] This invention belongs to the field of alloy materials technology, specifically relating to a nickel-based oxide dispersion-strengthened alloy material and its preparation method. Background Technology

[0002] Oxide dispersion strengthened nickel-based alloy MA754 is a novel high-temperature resistant material. It contains ultrafine oxide particles for dispersion strengthening and dispersed Cotillard atmospheres, forming an ultra-stable strengthened state with resistance to high-temperature creep. Compared to conventional high-temperature alloys without dispersed oxides, it exhibits superior high-temperature resistance when used in hot-end components in aero-engines and other equipment. With technological advancements, higher requirements are being placed on the service temperature of materials, necessitating the development of higher-performance high-temperature alloys.

[0003] Compared to typical high-temperature alloys, MA754 alloy possesses an oxide dispersion strengthening mechanism, resulting in superior mechanical properties. However, oxides tend to agglomerate at high temperatures, thereby disrupting the alloy's original unique composition and structure and reducing its mechanical properties. To ensure the dispersed distribution of oxides within the alloy, it is necessary to minimize the sintering temperature and shorten the holding time, enabling the material to meet the requirements of practical applications.

[0004] This invention utilizes a mixture of two alloy powders with different melting points. The high-melting-point alloy powder forms the framework of the joint region, while the low-melting-point alloy powder serves as the wetting phase. During the melting of the low-melting-point alloy, demelting elements B and Zr diffuse into the high-melting-point alloy, resulting in isothermal solidification during the holding stage. This lowers the sintering temperature and forms a solid solution with a relatively uniform microstructure and composition. Solid solution strengthening is achieved by utilizing the lattice distortion induced by Ti and Nb elements in the high-temperature alloy, and Ti is used to improve the alloy's oxidation resistance. SPS sintering allows for rapid heating and shorter holding times, further reducing oxide agglomeration at high temperatures. Under these process conditions, a nickel-based oxide dispersion-strengthened alloy material can be obtained. Summary of the Invention

[0005] In order to overcome the shortcomings and disadvantages of the prior art, the primary objective of this invention is to provide a nickel-based oxide dispersion-strengthened alloy material with a tensile strength of 935.57 to 951.88 MPa and a hardness of 329.47 to 356.05 HV.

[0006] Another objective of this invention is to provide a method for preparing nickel-based oxide dispersion-strengthened alloy materials, which employs high-energy ball milling and spark plasma sintering techniques.

[0007] The primary objective of this invention is achieved through the following technical solution:

[0008] A nickel-based oxide dispersion-reinforced alloy material is prepared by mixing two nickel-based alloy powders with different melting points. The specific compositions are as follows: the high-melting-point alloy powder comprises 74.1–77.1 wt.% nickel, 20 wt.% chromium, 0.5–2 wt.% titanium, 0.5–2 wt.% niobium, 1 wt.% iron, 0.3 wt.% aluminum, and 0.6 wt.% nano-yttrium oxide; the low-melting-point alloy powder comprises 77.6–79.6 wt.% nickel, 20 wt.% chromium, 6–8 wt.% zirconium, 2 wt.% boron, 1 wt.% iron, 0.5 wt.% titanium, 0.3 wt.% aluminum, and 0.6 wt.% nano-yttrium oxide. The low-melting-point alloy powder accounts for 1–3% of the total mass of the composite powder.

[0009] Preferably, the high-melting-point alloy powder in step (1) has the following composition: nickel 76.1 wt.%, chromium 20 wt.%, titanium 1 wt.%, niobium 1 wt.%, iron 1 wt.%, aluminum 0.3 wt.%, and nano-yttrium oxide 0.6 wt.%; the low-melting-point alloy powder has the following composition: nickel 68.6 wt.%, chromium 20 wt.%, zirconium 7 wt.%, boron 2 wt.%, iron 1 wt.%, titanium 0.5 wt.%, aluminum 0.3 wt.%, and nano-yttrium oxide 0.6 wt.%, and the low-melting-point alloy powder accounts for 3% of the total mass of the composite powder.

[0010] Preferably, the nickel-based oxide dispersion-strengthened alloy material has a tensile strength of 935.57–951.88 MPa and a hardness of 329.47–356.05 HV.

[0011] A method for preparing a nickel-based oxide dispersion-strengthened alloy material includes the following steps:

[0012] (1) Nickel powder, chromium powder, titanium powder, niobium powder, iron powder, aluminum powder and nano-yttrium oxide powder are subjected to high-energy ball milling and dried to obtain high-melting-point alloy powder; nickel powder, chromium powder, zirconium powder, boron powder, iron powder, titanium powder, aluminum powder and nano-yttrium oxide powder are subjected to high-energy ball milling and dried to obtain low-melting-point alloy powder; the ball-milled powder is dried and sieved to obtain powder with a particle size ≤15μm;

[0013] (2) The obtained high melting point alloy powder and low melting point alloy powder are mechanically mixed at a mass ratio of 1% to 3% of the low melting point alloy powder to obtain composite alloy powder;

[0014] (3) The composite alloy powder obtained in step (2) is subjected to discharge plasma sintering to obtain nickel-based oxide dispersion-strengthened alloy material.

[0015] Preferably, the drying temperature in step (1) is 60-80°C and the drying time is 12 hours.

[0016] Preferably, the specific conditions for high-energy ball milling in step (1) are as follows:

[0017] Speed: 300-400 rpm;

[0018] Ball to material ratio: 10:1;

[0019] A total of 3 kg of stainless steel grinding balls with diameters of 10 mm, 6 mm, and 3 mm were used, with a mass ratio of 1:3:1.

[0020] Ball mill atmosphere: Argon;

[0021] Ball milling time: 48-72 hours.

[0022] The stainless steel grinding balls used in this invention are of three different diameter types, all with the same density, and their quantity is determined by mass. For example, according to density = mass / volume, if there are 10 grinding balls with a diameter of 10mm weighing 100g, then there would be approximately 10 x (1000 / 216) grinding balls with a diameter of 6mm weighing 100g.

[0023] Preferably, the specific conditions for mechanical mixing in step (2) are as follows:

[0024] Speed: 100-120 rpm;

[0025] No stainless steel grinding balls added;

[0026] Mechanically mixed atmosphere: argon;

[0027] Mechanical mixing time: 12-24 hours.

[0028] Preferably, the specific sintering conditions in step (3) are as follows:

[0029] Sintering atmosphere: Vacuum;

[0030] Heating rate: 0-6 minutes: 100℃ / min; 6-11 minutes: 85℃ / min;

[0031] Sintering temperature: 1025~1050℃;

[0032] Keep warm for 10 minutes.

[0033] The present invention has the following advantages and beneficial effects compared with the prior art:

[0034] This invention prepares alloy powders with high and low melting points using high-energy ball milling to achieve uniform dispersion of elements. It utilizes the lattice distortion caused by titanium and niobium in the high-melting-point alloy powder to achieve solid solution strengthening, and titanium to improve the alloy's oxidation resistance. Boron and zirconium, demelting elements in the low-melting-point alloy powder, lower the sintering temperature of the nickel-based oxide dispersion-strengthened alloy material, preventing dispersion strengthening failure due to oxide agglomeration at high temperatures. The alloy powder is sintered using spark plasma, utilizing the diffusion of demelting elements from the low-melting-point alloy to the high-melting-point alloy during melting to achieve isothermal solidification, reducing the sintering temperature and shortening the holding time of the oxide dispersion-strengthened alloy. This avoids dispersion strengthening failure caused by oxide agglomeration at high temperatures and improves the alloy's mechanical properties. The prepared nickel-based oxide dispersion-strengthened alloy material exhibits a uniform distribution of oxide strengthening phases and high strength and hardness. Detailed Implementation

[0035] The present invention will be further described in detail below with reference to embodiments, but the implementation of the present invention is not limited thereto.

[0036] Example 1

[0037] A method for preparing a nickel-based oxide dispersion-strengthened alloy material includes the following steps:

[0038] (1) Weigh 228.3g of nickel powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 60g of chromium powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of titanium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of niobium powder (325 mesh, 99.95% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of iron powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 0.9g of aluminum powder (325 mesh, 99.7% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), and 1.8g of nano yttrium oxide powder (80nm, 99.9% purity, Chaowei Nano Co., Ltd.). Weighed metal powder was placed in a ball mill jar, vacuumed, and then filled with argon gas. High-energy ball milling was performed using a QM-2SP20-CL planetary ball mill (Nanjing University Instrument Factory) at a speed of 400 r / min for 48 h. Every 12 h, the ball mill jar was refilled with argon gas and the milling continued. The ball-to-powder ratio was 10:1. Three types of stainless steel grinding balls with diameters of 3 mm, 6 mm, and 10 mm, and masses of 600 g, 1800 g, and 600 g, respectively, were used. The mixed powder was then placed in a vacuum drying oven to remove moisture at 80 °C for 12 h to obtain high-melting-point alloy powder.

[0039] (2) Weigh out 235.8g of nickel powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 60g of chromium powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 21g of zirconium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 6g of boron powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of iron powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 1.5g of titanium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), and 0.9g of aluminum powder (325 mesh, 99.7% purity). Zhongnuo New Materials (Beijing) Technology Co., Ltd., 1.8g of nano-yttrium oxide powder (80nm, purity 99.9%, Chaowei Nano Co., Ltd.); The weighed metal powder was placed in a ball mill jar, vacuumed, and then filled with argon gas. High-energy ball milling was performed using a QM-2SP20-CL planetary ball mill (Nanjing University Instrument Factory). The ball milling speed was 400r / min, and the ball milling time was 48h. Every 12h, the ball mill jar was refilled with argon gas and the ball milling continued. The ball-to-powder ratio was 10:1, and the stainless steel grinding balls had diameters of 3mm, 6mm, and 10mm, with a mass ratio of 1:3:1. The mixed powder was placed in a vacuum drying oven to remove moisture at a temperature of 80℃ for 12h to obtain low-melting-point alloy powder.

[0040] (3) Weigh 97g of high melting point alloy powder and 3g of low melting point alloy powder, and mechanically mix them in a ball mill for 12h under an argon atmosphere, without adding stainless steel grinding balls, at a speed of 120rpm.

[0041] (4) Place the uniformly mixed composite powder into a vacuum drying oven to remove moisture at a temperature of 80°C for 12 hours to obtain dry composite metal powder.

[0042] (5) Weigh 20g of composite powder and place it in a mold for discharge plasma sintering. The external pressure is 40MPa and the sintering atmosphere is vacuum. The heating rate is 100℃ / min for 0-6 minutes and 85℃ / min for 6-11 minutes. Then, the sintering temperature is held at 1025℃ for 10 minutes and then cooled with the furnace.

[0043] The nickel-based oxide dispersion-strengthened alloy material described in this embodiment has a hardness of 356.05 HV and a tensile strength of 951.88 MPa according to the room temperature tensile test.

[0044] Example 2

[0045] A method for preparing a nickel-based oxide dispersion-strengthened alloy material includes the following steps:

[0046] (1) Weigh 228.3g of nickel powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 60g of chromium powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of titanium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of niobium powder (325 mesh, 99.95% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of iron powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 0.9g of aluminum powder (325 mesh, 99.7% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), and 1.8g of nano yttrium oxide powder (80nm, 99.9% purity, Chaowei Nano Co., Ltd.). Weighed metal powder was placed in a ball mill jar, vacuumed, and then filled with argon gas. High-energy ball milling was performed using a QM-2SP20-CL planetary ball mill (Nanjing University Instrument Factory) at a speed of 400 r / min for 48 h. Every 12 h, the ball mill jar was refilled with argon gas and the milling continued. The ball-to-powder ratio was 10:1, and the stainless steel grinding balls had diameters of 3 mm, 6 mm, and 10 mm, with a mass ratio of 1:3:1. The mixed powder was then placed in a vacuum drying oven to remove moisture at 80℃ for 12 h to obtain high-melting-point alloy powder.

[0047] (2) Weigh out 235.8g of nickel powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 60g of chromium powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 21g of zirconium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 6g of boron powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of iron powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), and 1.5g of titanium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.). The following materials were used: 0.9g aluminum powder (325 mesh, 99.7% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), and 1.8g nano yttrium oxide powder (80nm, 99.9% purity, Chaowei Nano Co., Ltd.). The weighed metal powders were placed in a ball mill jar, vacuumed, and then filled with argon gas. High-energy ball milling was performed using a QM-2SP20-CL planetary ball mill (Nanjing University Instrument Factory) at a speed of 400 r / min for 48 hours. Argon gas was refilled into the jar every 12 hours, and the ball-to-powder ratio was 10:1. The stainless steel grinding balls had diameters of 3mm, 6mm, and 10mm, with a mass ratio of 1:3:1. The mixed powder was then placed in a vacuum drying oven at 80℃ for 12 hours to remove moisture, yielding a low-melting-point alloy powder.

[0048] (3) Weigh 99g of high melting point alloy powder and 1g of low melting point alloy powder, and mechanically mix them in a ball mill for 12h under an argon atmosphere, without adding stainless steel grinding balls, at a speed of 120rpm.

[0049] (4) Place the uniformly mixed composite powder into a vacuum drying oven to remove moisture at a temperature of 80°C for 12 hours to obtain dry composite metal powder.

[0050] (5) Weigh 20g of composite powder and place it in a mold for discharge plasma sintering. The external pressure is 40MPa and the sintering atmosphere is vacuum. The heating rate is 100℃ / min for 0-6 minutes and 85℃ / min for 6-11 minutes. Then, the sintering temperature is held at 1025℃ for 10 minutes and then cooled with the furnace.

[0051] The nickel-based oxide dispersion-strengthened alloy material described in this embodiment has a hardness of 324.51 HV and a tensile strength of 887.40 MPa obtained from a room temperature tensile test.

[0052] Example 3

[0053] A method for preparing a nickel-based oxide dispersion-strengthened alloy material includes the following steps:

[0054] (1) Weigh 222.3g of nickel powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 60g of chromium powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 6g of titanium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 6g of niobium powder (325 mesh, 99.95% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of iron powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 0.9g of aluminum powder (325 mesh, 99.7% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), and 1.8g of nano yttrium oxide powder (80nm, 99.9% purity, Chaowei Nano Co., Ltd.). Weighed metal powder was placed in a ball mill jar, vacuumed, and then filled with argon gas. High-energy ball milling was performed using a QM-2SP20-CL planetary ball mill (Nanjing University Instrument Factory) at a speed of 400 r / min for 48 h. Every 12 h, the ball mill jar was refilled with argon gas and the milling continued. The ball-to-powder ratio was 10:1, and the stainless steel grinding balls had diameters of 3 mm, 6 mm, and 10 mm, with a mass ratio of 1:3:1. The mixed powder was then placed in a vacuum drying oven to remove moisture at 80℃ for 12 h to obtain high-melting-point alloy powder.

[0055] (2) Weigh out 235.8g of nickel powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 60g of chromium powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 21g of zirconium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 6g of boron powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of iron powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 1.5g of titanium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), and 0.9g of aluminum powder (325 mesh, 99.7% purity). Zhongnuo New Materials (Beijing) Technology Co., Ltd., 1.8g of nano-yttrium oxide powder (80nm, purity 99.9%, Chaowei Nano Co., Ltd.); The weighed metal powder was placed in a ball mill jar, vacuumed, and then filled with argon gas. High-energy ball milling was performed using a QM-2SP20-CL planetary ball mill (Nanjing University Instrument Factory). The ball milling speed was 400r / min, and the ball milling time was 48h. Every 12h, the ball mill jar was refilled with argon gas and the ball milling continued. The ball-to-powder ratio was 10:1, and the stainless steel grinding balls had diameters of 3mm, 6mm, and 10mm, with a mass ratio of 1:3:1. The mixed powder was placed in a vacuum drying oven to remove moisture at a temperature of 80℃ for 12h to obtain low-melting-point alloy powder.

[0056] (3) Weigh 97g of high melting point alloy powder and 3g of low melting point alloy powder, and mechanically mix them in a ball mill for 12h under an argon atmosphere, without adding stainless steel grinding balls, at a speed of 120rpm.

[0057] (4) Place the uniformly mixed composite powder into a vacuum drying oven to remove moisture at a temperature of 80°C for 12 hours to obtain dry composite metal powder.

[0058] (5) Weigh 20g of composite powder and place it in a mold for discharge plasma sintering. The external pressure is 40MPa and the sintering atmosphere is vacuum. The heating rate is 100℃ / min for 0-6 minutes and 85℃ / min for 6-11 minutes. Then, the sintering temperature is held at 1025℃ for 10 minutes and then cooled with the furnace.

[0059] The nickel-based oxide dispersion-strengthened alloy material described in this embodiment has a hardness of 316.84 HV and a tensile strength of 863.77 MPa obtained from a room temperature tensile test.

[0060] Comparative Example 1

[0061] A method for preparing a nickel-based oxide dispersion-strengthened alloy material includes the following steps:

[0062] (1) Weigh 228.3g of nickel powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 60g of chromium powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of titanium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of niobium powder (325 mesh, 99.95% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of iron powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 0.9g of aluminum powder (325 mesh, 99.7% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), and 1.8g of nano yttrium oxide powder (80nm, 99.9% purity, Chaowei Nano Co., Ltd.). Weighed metal powder was placed in a ball mill jar, vacuumed, and then filled with argon gas. High-energy ball milling was performed using a QM-2SP20-CL planetary ball mill (Nanjing University Instrument Factory) at a speed of 400 r / min for 48 h. Every 12 h, the ball mill jar was refilled with argon gas and the milling continued. The ball-to-powder ratio was 10:1, and the stainless steel grinding balls had diameters of 3 mm, 6 mm, and 10 mm, with a mass ratio of 1:3:1. The mixed powder was then placed in a vacuum drying oven to remove moisture at 80℃ for 12 h to obtain high-melting-point alloy powder.

[0063] (2) Weigh 100g of high melting point alloy powder, put it into a vacuum drying oven to remove moisture, the temperature is 80℃, the time is 12h, and dry high melting point alloy powder is obtained.

[0064] (3) Weigh 20g of high melting point alloy powder and place it in a mold for discharge plasma sintering. The external pressure is 40MPa, the sintering atmosphere is vacuum, the heating rate is 100℃ / min for 0-6 minutes, the heating rate is 85℃ / min for 6-11 minutes, and then the furnace is cooled after holding at 1025℃ for 10 minutes.

[0065] The nickel-based oxide dispersion-reinforced alloy material described in this comparative example has a measured hardness of 327.13 HV; the tensile strength obtained by room temperature tensile testing is 758.25 MPa. Compared with Example 1, the alloy material prepared in this comparative example has a much lower tensile strength than that of Example 1, even with only a slight difference in hardness.

[0066] Comparative Example 2

[0067] A method for preparing a nickel-based oxide dispersion-strengthened alloy material includes the following steps:

[0068] (1) Weigh 228.3g of nickel powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 60g of chromium powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of titanium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of niobium powder (325 mesh, 99.95% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of iron powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 0.9g of aluminum powder (325 mesh, 99.7% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), and 1.8g of nano yttrium oxide powder (80nm, 99.9% purity, Chaowei Nano Co., Ltd.). Weighed metal powder was placed in a ball mill jar, vacuumed, and then filled with argon gas. High-energy ball milling was performed using a QM-2SP20-CL planetary ball mill (Nanjing University Instrument Factory) at a speed of 400 r / min for 48 h. Every 12 h, the ball mill jar was refilled with argon gas and the milling continued. The ball-to-powder ratio was 10:1. Three types of stainless steel grinding balls with diameters of 3 mm, 6 mm, and 10 mm, and masses of 600 g, 1800 g, and 600 g, respectively, were used. The mixed powder was then placed in a vacuum drying oven to remove moisture at 80 °C for 12 h to obtain high-melting-point alloy powder.

[0069] (2) Weigh out 235.8g of nickel powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 60g of chromium powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 21g of zirconium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 6g of boron powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 3g of iron powder (325 mesh, 99.9% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), 1.5g of titanium powder (325 mesh, 99.5% purity, Zhongnuo New Materials (Beijing) Technology Co., Ltd.), and 0.9g of aluminum powder (325 mesh, 99.7% purity). Zhongnuo New Materials (Beijing) Technology Co., Ltd., 1.8g of nano-yttrium oxide powder (80nm, purity 99.9%, Chaowei Nano Co., Ltd.); The weighed metal powder was placed in a ball mill jar, vacuumed, and then filled with argon gas. High-energy ball milling was performed using a QM-2SP20-CL planetary ball mill (Nanjing University Instrument Factory). The ball milling speed was 400r / min, and the ball milling time was 48h. Every 12h, the ball mill jar was refilled with argon gas and the ball milling continued. The ball-to-powder ratio was 10:1, and the stainless steel grinding balls had diameters of 3mm, 6mm, and 10mm, with a mass ratio of 1:3:1. The mixed powder was placed in a vacuum drying oven to remove moisture at a temperature of 80℃ for 12h to obtain low-melting-point alloy powder.

[0070] (3) Weigh 97g of high melting point alloy powder and 3g of low melting point alloy powder, and mechanically mix them in a ball mill for 12h under an argon atmosphere, without adding stainless steel grinding balls, at a speed of 120rpm.

[0071] (4) Place the uniformly mixed composite powder into a vacuum drying oven to remove moisture at a temperature of 80°C for 12 hours to obtain dry composite metal powder.

[0072] (5) Weigh 20g of composite powder and place it in a mold for discharge plasma sintering. The external pressure is 40MPa and the sintering atmosphere is vacuum. The heating rate is 100℃ / min for 0-6 minutes and 85℃ / min for 6-11 minutes. Then, the sintering temperature is held at 1050℃ for 10 minutes and then cooled with the furnace.

[0073] The nickel-based oxide dispersion-strengthened alloy material described in this embodiment has a measured hardness of 318.18 HV; according to the room temperature tensile test, the tensile strength is 852.70 MPa. Compared with Example 1, the alloy material prepared in this comparative example has reduced hardness and tensile strength.

[0074] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.

Claims

1. A nickel-based oxide dispersion-strengthened alloy material, characterized in that, It is prepared by mixing two nickel-based alloy powders with different melting points; the specific composition is as follows: the high-melting-point alloy powder consists of nickel 74.1~77.1 wt.%, chromium 20 wt.%, titanium 0.5~2 wt.%, niobium 0.5~2 wt.%, iron 1 wt.%, aluminum 0.3 wt.%, and nano-yttrium oxide 0.6 wt.%; the low-melting-point alloy powder consists of nickel 77.6~79.6 wt.%, chromium 20 wt.%, zirconium 6~8 wt.%, boron 2 wt.%, iron 1 wt.%, titanium 0.5 wt.%, aluminum 0.3 wt.%, and nano-yttrium oxide 0.6 wt.%; the low-melting-point alloy powder accounts for 1~3% of the total alloy powder by mass. The preparation method of the nickel-based oxide dispersion-strengthened alloy material includes the following steps: (1) Nickel powder, chromium powder, titanium powder, niobium powder, iron powder, aluminum powder and nano-yttrium oxide powder are subjected to high-energy ball milling and dried to obtain high-melting-point alloy powder; nickel powder, chromium powder, zirconium powder, boron powder, iron powder, titanium powder, aluminum powder and nano-yttrium oxide powder are subjected to high-energy ball milling and dried to obtain low-melting-point alloy powder; the ball-milled powder is dried and sieved to obtain powder with a particle size ≤15μm; (2) The obtained high melting point alloy powder and low melting point alloy powder are ball-milled at a mass ratio of 97~99:1~3 to obtain composite alloy powder; (3) The composite alloy powder obtained in step (2) is subjected to discharge plasma sintering to obtain nickel-based oxide dispersion-strengthened alloy material.

2. The nickel-based oxide dispersion-strengthened alloy material according to claim 1, characterized in that, The high-melting-point alloy powder in step (1) consists of 76.1 wt.% nickel, 20 wt.% chromium, 0.5-2 wt.% titanium, 0.5-2 wt.% niobium, 1 wt.% iron, 0.3 wt.% aluminum, and 0.6 wt.% nano-yttrium oxide; the low-melting-point alloy powder consists of 78.6 wt.% nickel, 20 wt.% chromium, 6-8 wt.% zirconium, 2 wt.% boron, 1 wt.% iron, 0.5 wt.% titanium, 0.3 wt.% aluminum, and 0.6 wt.% nano-yttrium oxide, with the low-melting-point alloy powder accounting for 1-3% of the total alloy powder by mass.

3. The nickel-based oxide dispersion-strengthened alloy material according to claim 1, characterized in that, The nickel-based oxide dispersion-strengthened alloy material has a tensile strength of 935.57~951.88 MPa and a hardness of 329.47~356.05 HV.

4. A method for preparing a nickel-based oxide dispersion-strengthened alloy material according to any one of claims 1 to 3, characterized in that, Includes the following steps: (1) Nickel powder, chromium powder, titanium powder, niobium powder, iron powder, aluminum powder and nano-yttrium oxide powder are subjected to high-energy ball milling and dried to obtain high-melting-point alloy powder; nickel powder, chromium powder, zirconium powder, boron powder, iron powder, titanium powder, aluminum powder and nano-yttrium oxide powder are subjected to high-energy ball milling and dried to obtain low-melting-point alloy powder; the ball-milled powder is dried and sieved to obtain powder with a particle size ≤15μm; (2) The obtained high melting point alloy powder and low melting point alloy powder are ball-milled at a mass ratio of 97~99:1~3 to obtain composite alloy powder; (3) The composite alloy powder obtained in step (2) is subjected to discharge plasma sintering to obtain nickel-based oxide dispersion-strengthened alloy material.

5. The method for preparing nickel-based oxide dispersion-strengthened alloy materials according to claim 4, characterized in that, The drying temperature in step (1) is 60~80℃ and the time is 12h.

6. The method for preparing nickel-based oxide dispersion-strengthened alloy material according to claim 4, characterized in that, The specific conditions for high-energy ball milling in step (1) are as follows: Speed: 300~400 rpm; Ball to material ratio: 10:1; A total of 3 kg of stainless steel grinding balls with diameters of 10 mm, 6 mm, and 3 mm were used, with a mass ratio of 1:3:

1. Ball mill atmosphere: Argon; Ball milling time: 48~72h.

7. The method for preparing nickel-based oxide dispersion-strengthened alloy material according to claim 4, characterized in that, The specific conditions for high-energy ball milling in step (2) are as follows: Speed: 100~120 rpm; No stainless steel grinding balls added; Mechanically mixed atmosphere: argon; Mechanical mixing time: 12~24h.

8. The method for preparing nickel-based oxide dispersion-strengthened alloy material according to claim 4, characterized in that, The specific sintering conditions in step (3) are as follows: Sintering atmosphere: Vacuum; Heating rate: 0-6 minutes: 100℃ / min; 6-11 minutes: 85℃ / min; Sintering temperature: 1025~1050℃; Keep warm for 10 minutes.