阅读说明：本技术 高温合金的制备方法 (Preparation method of high-temperature alloy ) 是由 张瑞 崔传勇 周亦胄 孙晓峰 于 2020-07-01 设计创作，主要内容包括：本申请提供一种高温合金的制备方法,包括如下步骤：步骤(1)：将合金颗粒和氧化物粉末混合后进行球磨处理,获得球磨产物；步骤(2)：将球磨产物进行烧结致密,获得合金材料。根据本申请的高温合金的制备方法,能有效地提高合金中纳米氧化物的强化效果,实现强化合金的目的,使作为高温结构件的变形高温合金具备优异的抗氧化和抗蠕变性能。(The application provides a preparation method of a high-temperature alloy, which comprises the following steps: step (1): mixing alloy particles and oxide powder, and then carrying out ball milling treatment to obtain a ball-milled product; step (2): sintering and compacting the ball-milled product to obtain the alloy material. According to the preparation method of the high-temperature alloy, the strengthening effect of the nano oxide in the alloy can be effectively improved, the aim of strengthening the alloy is fulfilled, and the deformed high-temperature alloy serving as a high-temperature structural component has excellent oxidation resistance and creep resistance.)

1. The preparation method of the high-temperature alloy is characterized by comprising the following steps of:

step (1): mixing alloy particles and oxide powder, and then carrying out ball milling treatment to obtain a ball-milled product;

step (2): and sintering and compacting the ball-milled product to obtain the alloy material.

2. The method of preparing a superalloy as in claim 1, further comprising the steps of: carrying out thermal deformation treatment on the alloy material; a thermally deformable material is obtained.

3. The method of preparing a superalloy as in claim 2, further comprising the steps of: and carrying out heat treatment on the heat-deformed material to obtain a heat-treated material.

4. The method of claim 1, wherein the oxide is Y₂O₃、ThO₂、Al₂O₃MgO or a mixture thereof;

and/or, the oxide is a nanoscale oxide;

and/or the alloy particles are deformed superalloy particles;

and/or the alloy particles are spherical;

and/or the alloy particles have a particle size of d 1; wherein d1 is 10-900 μm;

and/or the particle size of the oxide is d 2; wherein d2<500 nm.

5. The method for preparing a superalloy as in claim 2, wherein the step of mixing the alloy particles and the oxide powder and then performing the ball milling process comprises the steps of:

putting alloy particles, oxide powder and grinding balls into a ball-milling tank in a vacuum environment for ball-milling treatment;

and/or the sintering equipment adopted for sintering and densifying is any one of vacuum hot-pressing sintering, spark plasma sintering and hot isostatic pressing sintering;

and/or the sintering temperature for sintering the compact is 1100-1300 ℃; and/or the sintering pressure is more than or equal to 25 MPa;

and/or the hot deformation treatment is any one of extrusion treatment, rolling treatment and die forging treatment;

and/or the thermal deformation temperature is 950-1200 ℃;

and/or, the sintering densification comprises the following steps: putting the ball-milled product into a graphite die, and then putting the graphite die into sintering equipment for hot-pressing sintering;

and/or, in the ball milling treatment process: the ball material ratio is 2:1-10: 1; and/or the ball milling rotating speed is 300-; and/or the ball milling time is 10-30 h.

6. The method of preparing a superalloy as in claim 1, wherein the method of preparing the alloy particles comprises the steps of:

s1: preparing a high-purity master alloy through duplex smelting or triple smelting of vacuum induction smelting and/or electroslag remelting and/or vacuum induction consumable smelting;

s2: high-temperature alloy particles are prepared by adopting a high-pressure gas atomization method.

7. The method of preparing a superalloy as in claim 3, wherein the wrought superalloy particles are any one of iron-based wrought superalloy particles, nickel-based wrought superalloy particles, and cobalt-based wrought superalloy particles;

and/or the wrought superalloy is a solid solution strengthened wrought superalloy.

8. The method of preparing a superalloy as in claim 3, wherein the wrought superalloy particles are any one of iron-based wrought superalloy particles, nickel-based wrought superalloy particles, and cobalt-based wrought superalloy particles;

and/or the wrought superalloy is a precipitation-hardening wrought superalloy.

9. The method of claim 7, wherein the heat treatment is solution treatment.

10. The method of claim 8, wherein the heat treatment is solution aging.

Technical Field

The application belongs to the technical field of alloy preparation, and particularly relates to a preparation method of a high-temperature alloy.

Background

At present, with the rapid development of the aerospace industry, the thrust-weight ratio of an aircraft is increased, the working temperature of engine parts is continuously increased, the research and development and application of high-temperature alloy are promoted, and a mode of adding strengthening elements into the alloy is often adopted for improving the performances of the high-temperature alloy, such as the heat strength, the oxidation resistance, the high-temperature endurance life and the like; or, an inert oxide reinforcing phase is introduced into the alloy by adopting a powder metallurgy method, and the oxide dispersion strengthened high-temperature alloy is prepared by high-energy ball milling and hot isostatic pressing or hot extrusion.

However, by adding the strengthening elements into the alloy, the phenomena of growth, raft or re-dissolution of precipitated phases in the high-temperature alloy can occur to some hot end parts of the aeroengine, such as a combustion chamber and a blade, along with the increase of the use temperature and the extension of the service time, the strengthening effect of the precipitated phases is reduced, and the service temperature and the service time of the deformed high-temperature alloy structural member are limited. And an inert oxide reinforcing phase is introduced into the alloy by adopting a powder metallurgy method, and the oxide dispersion strengthened high-temperature alloy (ODS) is prepared by high-energy ball milling and hot isostatic pressing or hot extrusion, and because the inert oxide has excellent thermal stability and chemical stability, the strengthening effect is still kept when the temperature is close to the melting point temperature of the high-temperature alloy, and the service temperature of the high-temperature alloy can be obviously improved. However, the addition of dispersion-strengthened phases to superalloys is also associated with the following problems: (1) the high-temperature alloy belongs to a material difficult to deform, the forming performance is poor, and the window of a hot processing process is small. After the dispersion strengthening phase is added, the deformation resistance is increased, so that the alloy deformation difficulty is higher, and a large-tonnage extruder is needed when the ODS is prepared; (2) the content of the oxide reinforcing phase is usually less than 2 wt.%, otherwise, agglomeration can occur, the plasticity of the alloy is reduced, the reinforcing phase becomes a weak part of the alloy, and holes are easy to aggregate to form a crack source during bearing; (3) in the process of preparing ODS by powder metallurgy, high-energy ball milling is needed to ensure that the reinforcing phase is fully dispersed and distributed, so that oxidation pollution is inevitably generated in the preparation process, and the ductility and toughness of the alloy are reduced; (4) ODS belongs to a discontinuous reinforced metal matrix composite, and according to Hashin-Shtrikman (H-S) equation calculation analysis, the composite with uniformly distributed reinforced phases corresponds to a lower limit model of material elastic modulus.

Therefore, how to provide a method for preparing a high-temperature alloy which can improve the strength without reducing the plasticity, improve the high-temperature deformation capacity of the material, improve the oxidation resistance and the high-temperature endurance life of the matrix high-temperature alloy, and strengthen the alloy is achieved, so that the deformed high-temperature alloy has excellent oxidation resistance and creep resistance, which is a problem to be solved by the technical personnel in the field.

Disclosure of Invention

Therefore, the technical problem to be solved by the present application is to provide a method for preparing a high temperature alloy, which can effectively improve the strengthening effect of nano oxides in the alloy, achieve the purpose of strengthening the alloy, and enable the deformed high temperature alloy as a high temperature structural member to have excellent oxidation resistance and creep resistance.

In order to solve the above problems, the present application provides a method for preparing a superalloy, comprising the steps of:

step (1): mixing alloy particles and oxide powder, and then carrying out ball milling treatment to obtain a ball-milled product;

step (2): sintering and compacting the ball-milled product to obtain the alloy material.

Preferably, the preparation method of the high-temperature alloy further comprises the following steps: carrying out thermal deformation treatment on the alloy material; a thermally deformable material is obtained.

Preferably, the preparation method of the high-temperature alloy further comprises the following steps: and carrying out heat treatment on the heat-deformed material to obtain a heat-treated material.

Preferably, the oxide is any one of Y2O3, ThO2, Al2O3 and MgO or any mixture thereof;

and/or the oxide is a nanoscale oxide;

and/or the alloy particles are deformed superalloy particles;

and/or the alloy particles are spherical;

and/or the alloy particles have a particle size d 1; wherein d1 is 10-900 μm;

and/or the particle size of the oxide is d 2; wherein d2<500 nm.

Preferably, the ball milling treatment after mixing the alloy particles and the oxide powder comprises the following steps:

putting alloy particles, oxide powder and grinding balls into a ball-milling tank in a vacuum environment for ball-milling treatment;

and/or the sintering equipment adopted for sintering and compacting is any one of vacuum hot-pressing sintering, spark plasma sintering and hot isostatic pressing sintering;

and/or the sintering temperature for sintering the compact is 1100-1300 ℃; and/or the sintering pressure is more than or equal to 25 MPa;

and/or the hot deformation treatment is any one of extrusion treatment, rolling treatment and die forging treatment;

and/or the thermal deformation temperature is 950-1200 ℃;

and/or, the sintering densification comprises the following steps: putting the ball-milled product into a graphite die, and then putting the graphite die into sintering equipment for hot-pressing sintering;

and/or, in the ball milling treatment process: the ball material ratio is 2:1-10: 1; and/or the ball milling rotating speed is 300-; and/or the ball milling time is 10-30 h.

Preferably, the preparation method of the alloy particles comprises the following steps:

s1: preparing a high-purity master alloy through duplex smelting or triple smelting of vacuum induction smelting and/or electroslag remelting and/or vacuum induction consumable smelting;

s2: high-temperature alloy particles are prepared by adopting a high-pressure gas atomization method.

Preferably, the wrought superalloy particles are any one of iron-based wrought superalloy particles, nickel-based wrought superalloy particles, and cobalt-based wrought superalloy particles;

and/or the wrought superalloy is a solid solution strengthened wrought superalloy.

Preferably, the wrought superalloy particles are any one of iron-based wrought superalloy particles, nickel-based wrought superalloy particles, and cobalt-based wrought superalloy particles;

and/or the wrought superalloy is a precipitation-hardening wrought superalloy.

Preferably, the heat treatment is solution treatment.

Preferably, the heat treatment mode is solution and aging treatment.

The application provides a preparation method of the high-temperature alloy; the area of the enrichment reinforcing phase forms a space net-shaped skeleton structure and wraps around the matrix alloy with toughness, the microstructure of the structure meets the material geometric structure of the upper limit value of the H-S theory, the elastic modulus and the strain energy storage of the material reach the theoretical upper limit, the connectivity between the matrixes is ensured, the strength can be improved without reducing the plasticity, the high-temperature deformation capacity of the material is improved, and the oxidation resistance and the high-temperature endurance life of the matrix high-temperature alloy are improved;

the nano-scale oxide in the alloy prepared by the method is distributed in a spatial network shape, so that the performances of high-temperature strength, creep resistance, oxidation resistance and the like of the alloy can be improved, the plasticity of the matrix alloy is kept, and the severe requirement of the subsequent thermal deformation of the alloy on the tonnage of equipment is reduced. The method optimizes the performance of the wrought superalloy by means of combining a powder metallurgy method and thermal mechanical treatment, realizes the purpose of shape control and property control cooperation, has less steps in the whole process, is simple to operate, and is a combination of traditional processing means; the invention does not introduce any chemical reagent and toxic and polluted gas, and has the advantage of environmental protection; the invention can achieve the purpose of near-net forming, improve the utilization rate of materials and reduce the subsequent machining cost. The performance of the part can be improved by adopting thermal deformation treatment and heat treatment;

during ball milling treatment, the ball milling rotating speed is low, the ball milling time is short, and the matrix particles are not ground, so that the method saves energy and improves the production efficiency; alloy particles, oxide powder and grinding balls are filled into a ball milling tank in a vacuum environment for ball milling treatment, so that the probability of introducing O, H and other gas impurities in the ball milling process is reduced;

performing thermal deformation treatment, and further deforming the sintered blank into a required part shape by using thermal processing equipment; the heat treatment can regulate and control the texture appearance of the alloy matrix, so that the mechanical property of the alloy is more excellent.

Drawings

FIG. 1 is a photograph of a superalloy powder according to the method of example 1 of the present invention.

FIG. 2 is a photograph of a mixed powder after ball milling according to the method described in example 1 of the present invention.

FIG. 3 is a photograph of the microstructure of the alloy after sintering according to the method of example 1 of the present invention.

FIG. 4 is a photograph of the microstructure of the alloy after deformation according to the method of example 1 of the present invention.

FIG. 5 is a photograph of the precipitated phases of the alloy matrix after heat treatment according to the method described in example 1 of the present invention.

Detailed Description

The preparation method of the high-temperature alloy in the embodiment comprises the following steps:

preparing a high-purity master alloy through duplex smelting or triple smelting of vacuum induction smelting and/or electroslag remelting and/or vacuum induction consumable smelting;

then preparing spherical high-temperature alloy particles by argon atomization;

putting the high-temperature alloy particles, the oxide powder, the grinding balls and the ball milling tank into a manual operation box, vacuumizing, closing a vacuum pump, filling argon, canning the high-temperature alloy particles, the oxide powder and the grinding balls when the internal pressure and the external pressure of the manual operation box are consistent, screwing down the ball milling tank, taking out the ball milling tank from the manual operation box, and installing the ball milling tank on a ball mill;

starting a ball mill to perform mixing ball milling, wherein the ball-material ratio is 2:1-10:1, the ball milling rotation speed is 300-600rad/min, the ball milling time is 10-30h, the ball milling rotation speed and the ball milling time are set according to the hardness of high-temperature alloy particles, oxide powder is uniformly embedded on the surfaces of the high-temperature particles during ball milling, the sizes of the high-temperature alloy particles are not obviously reduced, after the ball milling is finished, a ball milling tank is opened after being cooled to the room temperature, and the mixing material and the grinding balls are screened and separated;

putting the mixed material into a graphite mold, then putting the graphite mold into sintering equipment for hot-pressing sintering, wherein the sintering temperature is 1100-1300 ℃, the full compactness of the blank is ensured during sintering, and the blank is taken out after the blank is fully cooled after sintering;

thermally deforming the sintered blank at the thermal deformation temperature of 950-1200 ℃;

and finally, carrying out solid solution or solid solution aging treatment on the deformed alloy to obtain the nano-scale oxide reinforced high-temperature alloy with excellent structure performance.