CN118703815A - A nickel-based high-temperature alloy and a preparation method thereof - Google Patents
A nickel-based high-temperature alloy and a preparation method thereof Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
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- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
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- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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Abstract
本发明属于合金材料技术领域。更具体地，涉及一种镍基高温合金及其制备方法。本发明的制备方法包括：将氧化钇粉末和镍基合金粉末混合后，于惰性气体保护状态下，球磨混合均匀，以得到球磨料；其中，氧化钇粉末为单分散氧化钇粉末；单分散氧化钇粉末的D50为10‑11nm；单分散氧化钇粉末的粒径分布范围为5‑20nm；镍基合金粉末的D50为130‑140nm；镍基合金粉末的粒径分布范围为10‑280nm；并且，氧化钇粉末和所述镍基合金粉末的质量比为1：(100‑105)；将球磨料经真空除气后，热等静压烧结，以得到镍基合金块体；将镍基合金块体于室温条件下，进行旋锻，控制变形量为18‑20％，以得到冷变形加工料；将冷变形加工料于温度为850‑880℃条件下，保温1h退火处理，冷却，即得镍基高温合金。The present invention belongs to the technical field of alloy materials, and more specifically, relates to a nickel-based high-temperature alloy and a preparation method thereof. The preparation method of the present invention comprises: mixing yttrium oxide powder and nickel-based alloy powder, and then ball milling and mixing them uniformly under inert gas protection to obtain ball milling material; wherein the yttrium oxide powder is monodisperse yttrium oxide powder; the D50 of the monodisperse yttrium oxide powder is 10-11nm; the particle size distribution range of the monodisperse yttrium oxide powder is 5-20nm; the D50 of the nickel-based alloy powder is 130-140nm; the particle size distribution range of the nickel-based alloy powder is 10-280nm; and the mass ratio of the yttrium oxide powder to the nickel-based alloy powder is 1:(100-105); vacuum degassing the ball milling material, hot isostatic pressing and sintering to obtain a nickel-based alloy block; rotary forging the nickel-based alloy block at room temperature to control the deformation amount to 18-20% to obtain a cold deformation processing material; annealing the cold deformation processing material at a temperature of 850-880°C for 1h, cooling, and obtaining a nickel-based high-temperature alloy.
Description
Technical Field
The invention belongs to the technical field of alloy materials. More particularly, to a nickel-based superalloy and a method of making the same.
Background
The nickel-base superalloy is an alloy which uses nickel as a matrix and can resist oxidation or corrosive media at a high temperature of 600 ℃ or higher. Such alloys are key materials for the manufacture of high temperature components for aircraft engines, industrial gas turbines, nuclear reactors, and the like.
Among these, there is a type of nickel-based superalloy, which is generally called a nickel-based oxide dispersion strengthened alloy (ODS alloy), by introducing ultrafine oxide particles such as yttria into an alloy matrix to improve the high temperature strength and creep resistance of an alloy product.
In the case of an ODS alloy, during processing, the migration of grain boundaries and the rapid diffusion of elements in the vicinity of the grain boundaries tend to cause dissolution of oxide particles in response to the migration of the grain boundaries, and grain boundary-free zones are formed. As the oxide particles dissolve gradually, elements near the grain boundaries are enriched, and when the content exceeds the solubility of the alloy elements by the grain boundaries, part of the oxide particles are re-precipitated and the oxide particles grow up through Ostwald ripening. In the cold deformation process, the alloy and the matrix have good coherent relation, oxide particles coarsen, so that the coherent relation with the matrix is slowly lost, in the heat treatment process, if the temperature is too high, the coarsen oxide particles further grow up, the dislocation density in the alloy also increases, the strengthening effect is achieved, and meanwhile, the plasticity and toughness of the alloy are obviously reduced.
However, due to the growth of crystal grains or the effect of secondary recrystallization, a part of the nano oxide positioned at the crystal boundary is a coherent interface with the alloy matrix, and the other part of the nano oxide is a non-coherent interface, so that the interface energy of the non-coherent part is increased, oxide particles grow up and the shape is changed, the microstructure of the product is degraded, and the strength of the product is reduced.
Disclosure of Invention
The invention aims to solve the technical problems that: aiming at the problem that the high-temperature strength of an alloy product is reduced due to overlarge oxide particles or shape change caused by grain growth or secondary recrystallization in the preparation process of the nickel-based superalloy, the invention provides the nickel-based superalloy and a preparation method thereof.
The invention aims to provide a nickel-based superalloy.
Another object of the invention is to provide a method for preparing a nickel-base superalloy.
The above object of the present invention is achieved by the following technical scheme:
the preparation method of the nickel-based superalloy comprises the following specific preparation steps:
Raw material preparation:
mixing yttrium oxide powder and nickel-based alloy powder, and then ball-milling and uniformly mixing under the protection of inert gas to obtain a ball abrasive;
Wherein the yttrium oxide powder is monodisperse yttrium oxide powder; the D50 of the monodisperse yttrium oxide powder is 10-11nm; the particle size distribution range of the monodisperse yttrium oxide powder is 5-20nm;
The D50 of the nickel-based alloy powder is 130-140nm; the particle size distribution range of the nickel-based alloy powder is 10-280nm;
And, the mass ratio of the yttrium oxide powder to the nickel-based alloy powder is 1: (100-105);
sintering materials:
Carrying out vacuum degassing on the ball abrasive, and carrying out hot isostatic pressing sintering to obtain a nickel-based alloy block;
forging at room temperature:
performing rotary forging on the nickel-based alloy block under the room temperature condition, and controlling the deformation amount to be 18-20% so as to obtain a cold deformation processing material;
Annealing:
and (3) carrying out heat preservation on the cold deformation processing material for 1h at the temperature of 850-880 ℃ for annealing treatment, and cooling to obtain the nickel-based superalloy.
According to the technical scheme, the monodisperse nano yttrium oxide powder is adopted in the nickel-based alloy powder system, so that monodisperse oxide particles can be more uniformly distributed in an alloy matrix, on one hand, the need for adjusting the particle distribution in the preparation process is reduced, and the need for ball milling mixing time can be shortened to a certain extent, so that excessive agglomeration of the particles under the action force of mechanical ball milling can be avoided; on the other hand, oxide particles with more uniform particle size distribution can obviously reduce the growth rate difference among different particles in the processing process, thereby being beneficial to controlling the coarsening process of the particles at high temperature and improving the uniformity of the microstructure of the alloy; furthermore, the monodisperse fine oxide particles can be used as barriers for grain growth, maintain the fine grain structure of the alloy and improve the high-temperature strength and creep resistance of the alloy.
Further, the sphericity of the yttrium oxide powder is 9.0-9.5.
By further adopting the above oxide powder of higher sphericity, first, the particles of higher sphericity will cause a more uniform local stress distribution in the adoption, thereby helping to reduce the non-uniformity in the grain growth process due to stress concentration; secondly, the interface stress of the spherical particles is lower, so that the non-uniform grain growth caused by non-uniform interface stress or the generation of internal microcracks and the like can be reduced; furthermore, due to the geometrical characteristics of the particles with higher sphericity, coarsening of crystal grains caused by concentration of thermal stress can be remarkably reduced, so that the high-temperature strength of the product is further improved.
Further, the hot isostatic pressing comprises:
And (3) continuously performing hot isostatic pressing sintering for 3-3.2h under the conditions that the temperature is 1180-1200 ℃ and the pressure is 168-170 MPa.
Further, the sintering of the material further comprises:
Heating at a speed of 6-8 ℃/min to 750-800 ℃, continuously heating at a speed of 0.5-0.7 ℃/min to 1180-1200 ℃, continuously performing hot isostatic pressing sintering for 3-3.2h under the condition of 168-170MPa, subsequently cooling at a speed of 8-12 ℃/min to 550-600 ℃, and continuously cooling at a speed of 2-4 ℃/min to room temperature.
According to the technical scheme, the heating rate and the cooling rate in the heating process are further controlled, so that the phenomenon that a large temperature difference is generated between the surface and the inside of a material due to the excessively high heating rate in the heating process is avoided, uneven thermal stress is caused, and finally inconsistent microstructures are caused, so that the high-temperature strength of a product is reduced; in the cooling process, a finer grain structure can be obtained by increasing the cooling speed, but higher residual stress is easy to cause, so that the cooling speed needs to be reasonably controlled.
Further, the nickel-based alloy powder comprises the following elements in parts by weight:
18-20 parts of Cr,0.6-0.7 part of Ti,0.25-0.28 part of Al,0.9-1.0 part of Fe,0.04-0.05 part of C and 80-82 parts of Ni.
Further, the ball milling and mixing uniformly comprises:
Taking the total mass of the yttrium oxide powder and the nickel-based alloy powder as the mass of the materials, and according to the mass ratio of ball milling beads to the mass of the materials, the mass ratio is 35:1 adding zirconia ball milling beads, wherein the zirconia ball milling beads adopt three specifications with diameters of 3cm, 5cm and 8cm respectively; wherein, the number ratio of 3cm ball-milling beads, 5cm ball-milling beads and 8cm ball-milling beads is 8:5:2;
ball milling and mixing for 20min under the condition that the rotation speed is 320r/min and the revolution speed is 450 r/min.
The nickel-based superalloy is prepared by the preparation method.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Reagents and materials used in the following examples are commercially available unless otherwise specified.
Example 1
Raw material preparation:
mixing yttrium oxide powder and nickel-based alloy powder, and then ball-milling and uniformly mixing under the protection of argon gas to obtain a ball abrasive;
the ball milling and mixing uniformly comprises the following steps:
Taking the total mass of the yttrium oxide powder and the nickel-based alloy powder as the mass of the materials, and according to the mass ratio of ball milling beads to the mass of the materials, the mass ratio is 35:1 adding zirconia ball milling beads, wherein the zirconia ball milling beads adopt three specifications with diameters of 3cm, 5cm and 8cm respectively; wherein, the number ratio of 3cm ball-milling beads, 5cm ball-milling beads and 8cm ball-milling beads is 8:5:2;
ball milling and mixing for 20min under the condition that the rotation speed is 320r/min and the revolution speed is 450 r/min;
wherein the yttrium oxide powder is monodisperse yttrium oxide powder; the D50 of the monodisperse yttrium oxide powder is 10nm; the particle size distribution range of the monodisperse yttrium oxide powder is 5-20nm;
the sphericity of the yttrium oxide powder is 9.0;
The D50 of the nickel-based alloy powder is 130nm; the particle size distribution range of the nickel-based alloy powder is 10-280nm;
And, the mass ratio of the yttrium oxide powder to the nickel-based alloy powder is 1:100;
The nickel-based alloy powder comprises the following elements in parts by weight:
18 parts of Cr,0.6 part of Ti,0.25 part of Al,0.9 part of Fe,0.04 part of C and 80 parts of Ni;
sintering materials:
Heating the ball abrasive material to 750 ℃ at a speed of 6 ℃/min after vacuum degassing, continuously heating to 1180 ℃ at a speed of 0.5 ℃/min, continuously performing hot isostatic pressing sintering for 3 hours under the condition that the pressure is 168MPa, continuously cooling to 550 ℃ at a speed of 8 ℃/min, and continuously cooling to room temperature at a speed of 2 ℃/min to obtain a nickel-based alloy block;
forging at room temperature:
Performing rotary forging on the nickel-based alloy block under the room temperature condition, and controlling the deformation amount to be 18% so as to obtain a cold deformation processing material;
Annealing:
and (3) carrying out heat preservation on the cold deformation processing material for 1h at the temperature of 850 ℃ for annealing treatment, and cooling to obtain the nickel-based superalloy.
Example 2
Raw material preparation:
mixing yttrium oxide powder and nickel-based alloy powder, and then ball-milling and uniformly mixing under the protection of argon gas to obtain a ball abrasive;
the ball milling and mixing uniformly comprises the following steps:
Taking the total mass of the yttrium oxide powder and the nickel-based alloy powder as the mass of the materials, and according to the mass ratio of ball milling beads to the mass of the materials, the mass ratio is 35:1 adding zirconia ball milling beads, wherein the zirconia ball milling beads adopt three specifications with diameters of 3cm, 5cm and 8cm respectively; wherein, the number ratio of 3cm ball-milling beads, 5cm ball-milling beads and 8cm ball-milling beads is 8:5:2;
ball milling and mixing for 20min under the condition that the rotation speed is 320r/min and the revolution speed is 450 r/min;
Wherein the yttrium oxide powder is monodisperse yttrium oxide powder; the D50 of the monodisperse yttrium oxide powder is 10.5nm; the particle size distribution range of the monodisperse yttrium oxide powder is 5-20nm;
the sphericity of the yttrium oxide powder is 9.3;
The D50 of the nickel-based alloy powder is 135nm; the particle size distribution range of the nickel-based alloy powder is 10-280nm;
And, the mass ratio of the yttrium oxide powder to the nickel-based alloy powder is 1:102, a step of;
The nickel-based alloy powder comprises the following elements in parts by weight:
19 parts of Cr,0.6 part of Ti,0.26 part of Al,0.9 part of Fe,0.04 part of C and 80 parts of Ni;
sintering materials:
Heating the ball abrasive material to 780 ℃ at a speed of 7 ℃/min after vacuum degassing, continuously heating to 1190 ℃ at a speed of 0.6 ℃/min, continuously performing hot isostatic pressing sintering for 3.1h under the condition of 169MPa, and continuously cooling to room temperature at a speed of 3 ℃/min after cooling to 580 ℃ at a speed of 10 ℃/min to obtain a nickel-based alloy block;
forging at room temperature:
performing rotary forging on the nickel-based alloy block under the room temperature condition, and controlling the deformation amount to be 19% so as to obtain a cold deformation processing material;
Annealing:
and (3) carrying out heat preservation on the cold deformation processing material for 1h under the condition that the temperature is 860 ℃ for annealing treatment, and cooling to obtain the nickel-based superalloy.
Example 3
Raw material preparation:
mixing yttrium oxide powder and nickel-based alloy powder, and then ball-milling and uniformly mixing under the protection of argon gas to obtain a ball abrasive;
the ball milling and mixing uniformly comprises the following steps:
Taking the total mass of the yttrium oxide powder and the nickel-based alloy powder as the mass of the materials, and according to the mass ratio of ball milling beads to the mass of the materials, the mass ratio is 35:1 adding zirconia ball milling beads, wherein the zirconia ball milling beads adopt three specifications with diameters of 3cm, 5cm and 8cm respectively; wherein, the number ratio of 3cm ball-milling beads, 5cm ball-milling beads and 8cm ball-milling beads is 8:5:2;
ball milling and mixing for 20min under the condition that the rotation speed is 320r/min and the revolution speed is 450 r/min;
Wherein the yttrium oxide powder is monodisperse yttrium oxide powder; the D50 of the monodisperse yttrium oxide powder is 11nm; the particle size distribution range of the monodisperse yttrium oxide powder is 5-20nm;
the sphericity of the yttrium oxide powder is 9.5;
The D50 of the nickel-based alloy powder is 140nm; the particle size distribution range of the nickel-based alloy powder is 10-280nm;
And, the mass ratio of the yttrium oxide powder to the nickel-based alloy powder is 1:105;
The nickel-based alloy powder comprises the following elements in parts by weight:
20 parts of Cr,0.7 part of Ti,0.28 part of Al,1.0 part of Fe,0.05 part of C and 82 parts of Ni;
sintering materials:
Heating the ball abrasive material to 800 ℃ at a speed of 8 ℃/min after vacuum degassing, continuously heating to 1200 ℃ at a speed of 0.7 ℃/min, continuously performing hot isostatic pressing sintering for 3.2 hours under the condition of 170MPa, continuously cooling to 600 ℃ at a speed of 12 ℃/min, and continuously cooling to room temperature at a speed of 4 ℃/min to obtain a nickel-based alloy block;
forging at room temperature:
Performing rotary forging on the nickel-based alloy block under the room temperature condition, and controlling the deformation amount to be 20% so as to obtain a cold deformation processing material;
Annealing:
and (3) carrying out heat preservation on the cold deformation processing material for 1h annealing treatment at the temperature of 880 ℃ and cooling to obtain the nickel-based superalloy.
Example 4
The difference between this embodiment and embodiment 1 is that: the sphericity of the yttria powder was 8.8, the remaining conditions remained unchanged.
Example 5
The difference between this embodiment and embodiment 1 is that: the temperature rising rates of the materials during sintering are different, and specifically:
sintering materials:
Heating the ball abrasive material to 1180 ℃ at a speed of 6 ℃/min after vacuum degassing, continuously performing hot isostatic pressing sintering for 3 hours under the condition of 168MPa, and continuously cooling to room temperature at a speed of 2 ℃/min after cooling to 550 ℃ at a speed of 8 ℃/min to obtain the nickel-based alloy block.
Example 6
The difference between this embodiment and embodiment 1 is that: the material sintering temperature reduction rates are different, and specifically:
sintering materials:
Heating the ball abrasive material to 750 ℃ at a speed of 6 ℃/min after vacuum degassing, continuously heating to 1180 ℃ at a speed of 0.5 ℃/min, continuously performing hot isostatic pressing sintering for 3 hours under the condition of 168MPa, and then cooling to room temperature at a speed of 2 ℃/min to obtain the nickel-based alloy block.
Comparative example 1
The difference between this comparative example and example 1 is that:
The yttrium oxide powder is non-monodisperse yttrium oxide powder; the D50 of the monodisperse yttrium oxide powder is 10nm; the particle size distribution range of the monodisperse yttrium oxide powder is 0.5-60nm.
Comparative example 2
The difference between this comparative example and example 1 is that:
The yttrium oxide powder is non-monodisperse yttrium oxide powder; the D50 of the monodisperse yttrium oxide powder is 80nm; the particle size distribution range of the monodisperse yttrium oxide powder is 1-160nm.
The products obtained in examples 1-6 and comparative examples 1-2 were subjected to performance tests, and specific test methods and test results are as follows:
And (3) polishing the sample by using No. 2000 sand paper, and carrying out a stretching experiment on the polished stretching strip sample in an Instron 5585H laser induced stretching experiment machine, wherein the testing temperature is from room temperature to 700 ℃, and the strain rate is 1 multiplied by 10 -3S-1.
In the above manner, the yield strength and ultimate tensile strength of the sample at room temperature and at 700 ℃ were respectively obtained, and the detailed test results are shown in table 1;
table 1: product performance test results
From the test results in Table 1, it can be seen that the product of the present invention can have a beneficial high temperature strength.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (7)
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