CN115261753A - Hot working method for producing high-uniformity ultra-fine grain nickel-based high-temperature alloy - Google Patents

Hot working method for producing high-uniformity ultra-fine grain nickel-based high-temperature alloy Download PDF

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CN115261753A
CN115261753A CN202110471311.6A CN202110471311A CN115261753A CN 115261753 A CN115261753 A CN 115261753A CN 202110471311 A CN202110471311 A CN 202110471311A CN 115261753 A CN115261753 A CN 115261753A
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nickel
temperature
ultra
hot working
working method
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张健杨
孙明月
徐斌
李殿中
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Institute of Metal Research of CAS
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon

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Abstract

The invention relates to the field of hot working of nickel-based high-temperature alloy, in particular to a hot working method for producing high-uniformity ultra-fine grain nickel-based high-temperature alloy, which can be used in the field of high-temperature alloy forging. The method comprises the following process steps: firstly, putting a nickel-based high-temperature alloy forging into a heating furnace to be heated to 700-750 ℃, and preserving heat for a period of time; then heating the high-temperature alloy to 850-950 ℃, and preserving the heat for a period of time; continuously heating the high-temperature alloy to 950-1020 ℃, and preserving the temperature for a period of time; and finally, taking out the high-temperature alloy, and carrying out upsetting, drawing, extruding or die forging forming, wherein the total deformation is controlled to be more than 40%. The structure refining process of the nickel-based superalloy is simple, a step heating process is adopted for 3 times in the temperature rising process, precipitated phases are uniformly distributed by regulating and controlling the precipitated phase precipitation sequence in the alloy, and the problem that coarse crystals and mixed crystals in the nickel-based superalloy cannot be eliminated by the traditional forging process at present is solved.

Description

Hot working method for producing high-uniformity ultra-fine grain nickel-based high-temperature alloy
Technical Field
The invention relates to the field of hot working of nickel-based high-temperature alloy, in particular to a hot working method for producing high-uniformity ultra-fine grain nickel-based high-temperature alloy, which can be used in the field of high-temperature alloy forging.
Background
During the conventional hot deformation of GH4169 ingots to bars, a hot working Process known as Delta Process (DP) successfully eliminates the occasional presence of large grains and effectively refines the grains. In this process, intentional precipitation of the delta phase and subsequent thermomechanical processing is used to produce uniform, fine-grained bar stock. At present, GH4169 alloy turbine disk forgings with the grain size grade of more than 8 grade can be obtained through the DP process, but because more delta phase is precipitated by the DP process, a large amount of flaky delta phase still exists in the alloy after the alloy is in a hot state, and the excessive delta phase serving as a crack initiation and development channel can reduce the strength of the alloy. And the DP process needs aging for 24 hours or more at about 900 ℃, and long-time aging treatment causes the delta phase to be easy to aggregate and precipitate at the grain boundary, which not only easily causes the distribution of the precipitated phase in the structure to be uneven, but also causes Nb element to be enriched at the grain boundary to cause the alloy composition to be uneven, and uniform and fine grains are difficult to obtain in the subsequent hot deformation process.
Disclosure of Invention
The invention aims to provide a hot working method for producing high-uniformity ultra-fine grain nickel-based high-temperature alloy, which obtains a uniformly distributed delta phase by a method of converting a high-temperature gamma' phase into the delta phase and is used for solving the problem of uneven grain size distribution after hot working due to the fact that the delta phase is easy to segregate in a grain boundary when being directly precipitated.
The technical scheme of the invention is as follows:
a hot working method for producing high-uniformity ultra-fine grained nickel-based superalloy comprises the following process steps:
1) Putting the nickel-based high-temperature alloy forging into a heating furnace, heating to 700-750 ℃, preserving heat for 5-10 h, and uniformly separating out a gamma' phase;
2) Heating the nickel-based high-temperature alloy treated in the step 1) to 850-950 ℃, and preserving the heat for 5-10 h to convert a gamma' phase into a delta phase;
3) Heating the nickel-based high-temperature alloy treated in the step 2) to 950-1020 ℃, and preserving the heat for 5 min-2 h;
4) And (3) carrying out upsetting-drawing, extruding or die forging forming on the nickel-based high-temperature alloy treated in the step 3), wherein the total deformation is controlled to be more than 40%.
The hot working method for producing the high-uniformity ultra-fine grain nickel-based high-temperature alloy comprises the following steps of 1), selecting the heat preservation temperature of 720 ℃, and preserving the heat for 8 hours to ensure that the volume fraction content of a gamma' phase in a structure reaches 50-80%.
The hot working method for producing the high-uniformity ultra-fine grain nickel-based high-temperature alloy comprises the following steps of 2) selecting the heat preservation temperature of 900 ℃ and preserving the heat for 8 hours to ensure that the volume fraction content of the delta phase reaches 60-90%.
The hot working method for producing the high-uniformity ultra-fine grain nickel-based high-temperature alloy comprises the step 3) of selecting the heat preservation temperature of 960 ℃ and preserving the heat for 1 hour to ensure that the volume fraction content of the delta phase is remained by 40-60%.
The hot processing method for producing the high-uniformity ultrafine-grained nickel-based high-temperature alloy comprises the steps of 1), 2) and 3), wherein the nickel-based high-temperature alloy is placed into a heat treatment furnace, timing is started after the temperature is increased to a set temperature and is kept for 10min, and the temperature increase rate is not higher than 200 ℃/h.
The hot processing method for producing the high-uniformity ultra-fine grain nickel-based high-temperature alloy is continuously implemented among the step 1), the step 2) and the step 3), and the heating rate is not higher than 200 ℃/h.
In the hot working method for producing the high-uniformity ultra-fine grained nickel-based high-temperature alloy, the step 4) is preferably performed by 1 heating, and the total deformation is controlled to be 40%.
The hot working method for producing the high-uniformity ultrafine-grained nickel-based high-temperature alloy is used for obtaining the nickel-based high-temperature alloy with uniform ultrafine-grained structure, and the grain size of the nickel-based high-temperature alloy is 8-10 grades.
The design idea of the invention is as follows:
the invention provides a hot working method for producing high-uniformity ultra-fine grain nickel-based high-temperature alloy, which creatively introduces that the alloy is kept warm for 8 hours at 720 ℃, and the precipitation mode of a delta phase is changed from direct precipitation from austenite to conversion from a gamma' phase to the delta phase. Therefore, on the premise of ensuring the mass fraction of the delta phase, the delta phase which is uniformly distributed is obtained, and the effect of promoting recrystallization nucleation of the delta phase in the thermal deformation process is utilized, so that the effective grain refinement is ensured.
The invention has the advantages and beneficial effects that:
the nickel-based superalloy structure refining process is simple, a step heating process is adopted for 3 times in the temperature rising process, precipitated phases are uniformly distributed by regulating and controlling the precipitation sequence of the precipitated phases in the alloy, and the uniformly distributed precipitated phases can provide recrystallization nucleation positions and increase the nucleation rate in the hot working forging process; secondly, the crystal boundary can be pinned, the movement of the crystal boundary is hindered, and the growth speed of the crystal grain is reduced, so that the high-temperature alloy with uniform ultrafine grain structure is obtained.
Drawings
Fig. 1 is a metallographic picture obtained in example 1.
Fig. 2 is a metallographic picture obtained in comparative example 1.
Detailed Description
In the specific implementation process, the hot working method for producing the high-uniformity ultra-fine grained nickel-based superalloy, disclosed by the invention, comprises the steps of 1) uniformly precipitating gamma ', 2) converting a gamma' phase into a delta phase, and 3) controlling the thermal deformation of a structure containing the delta phase. Firstly, heating the material to 700-750 ℃, and preserving heat for 5-10 h to obtain the nickel-based high-temperature alloy with fine and uniformly distributed gamma' phase particles. Then, the nickel-based high-temperature alloy is placed in a heat treatment furnace, the temperature of the heat treatment furnace is raised to 850-950 ℃, and the temperature is kept for 5-10 hours, so that the uniformly distributed gamma' phase is converted into a stable and uniformly distributed delta phase. Finally, the temperature is kept at 950-1020 ℃ for 0.5-2 h, and deformation (such as upsetting, extruding or die forging forming) is carried out, so that the problem that the delta phase is completely dissolved due to overhigh temperature is solved. The total deformation is controlled to be more than 40 percent, and the deformation is prevented from being too small to achieve the thinning effect.
Preferably, the temperature of step 1) 700-750 ℃ in the heat treatment process is the precipitation temperature of gamma ', and a uniform and fine gamma' phase can be obtained by selecting 720 ℃ and keeping the temperature for 8 h. Step 2) in the heat treatment process, the temperature of 850-950 ℃ is within the delta phase transition temperature range, and the transition peak is selected when the temperature is maintained at 900 ℃ for 8 h. Step 3) 950-1020 ℃ in the heat treatment process is an optimal deformation temperature range, and more delta phase can be reserved by selecting 960 ℃ for heat preservation for 1 h.
The present invention will be explained in further detail below by way of examples and figures.
Example 1
In this embodiment, the hot working method for producing the high-uniformity ultra-grain-refining GH4169 alloy includes the following steps:
(1) Processing the alloy to be processed into a phi 8X 12mm sample, putting the processed sample into a heat treatment furnace, preserving heat for 8h at 720 ℃, timing after the temperature is raised to a set temperature and preserved for 10min, wherein the temperature raising rate is 50 ℃/h, and the volume fraction content of a gamma' phase in a tissue reaches 80%.
(2) And (2) preserving the temperature of the sample treated in the step (1) at 900 ℃ for 8h, beginning timing after the temperature is raised to the set temperature and preserved for 10min, wherein the temperature rise rate is 100 ℃/h, and the volume fraction content of the delta phase reaches 80%.
(3) And (3) heating the sample treated in the step (2) to 960 ℃, preserving heat for 1h, starting timing after the temperature is increased to the set temperature and preserved for 10min, wherein the heating rate is 150 ℃/h, and the volume fraction content of the delta phase is left by 50%.
(4) Upsetting the sample treated in the step (3), and forming the sample to the height of 6mm by 1 heating.
As shown in figure 1, the processed sample is subjected to mechanical polishing and chemical corrosion, the metallographic structure is observed, the grains are fine and uniform, no coarse grains exist, the grain size reaches 8 grades, and a small amount of delta phase is contained.
Comparative example 1
In the comparative example, the hot working method for GH4169 alloy grain refinement comprises the following steps:
(1) Processing the alloy to be treated into a sample with the diameter of 8 mm multiplied by 12mm, and preserving the temperature of the processed sample at 900 ℃ for 24h.
(2) And (2) heating the sample treated in the step (1) to 950 ℃, preserving the heat for 5 mm, and then deforming to 6mm.
As shown in FIG. 2, the treated sample was subjected to mechanical polishing and chemical etching to observe the metallographic structure, and the grain size distribution was not uniform, and still contained coarse grains and a large amount of undissolved delta phase.
In the preparation methods of example 1 and comparative example 1, the GH4169 alloy blank material can be prepared according to the methods for preparing GH4169 alloy disclosed in the prior art, and can also be obtained commercially.
The results of the embodiment and the comparative example show that compared with the traditional method for directly precipitating the delta phase, the method for obtaining the delta phase by the phase-to-phase conversion of the high-temperature gamma' has more advantages in the aspect of grain refinement, and solves the problem that the conventional forging process cannot eliminate coarse crystals and mixed crystals in the nickel-based high-temperature alloy.

Claims (8)

1. A hot working method for producing high-uniformity ultra-fine grain nickel-based superalloy is characterized by comprising the following process steps:
1) Putting the nickel-based high-temperature alloy forging into a heating furnace, heating to 700-750 ℃, preserving heat for 5-10 h, and uniformly separating out a gamma' phase;
2) Heating the nickel-based high-temperature alloy treated in the step 1) to 850-950 ℃, and preserving the heat for 5-10 hours to convert a gamma' phase into a delta phase;
3) Heating the nickel-based high-temperature alloy treated in the step 2) to 950-1020 ℃, and preserving the heat for 5 min-2 h;
4) Upsetting, drawing, extruding or die forging the nickel-base superalloy treated in the step 3), wherein the total deformation is controlled to be more than 40%.
2. The hot working method for producing high-uniformity ultra-fine grained nickel-based superalloy according to the claim 1, wherein the heat preservation temperature in the step 1) is 720 ℃, and the heat preservation time is 8 hours, so that the volume fraction content of the gamma' phase in the structure is 50-80%.
3. The hot working method for producing high-uniformity ultra-fine grained nickel-based superalloy according to the claim 1, wherein the temperature of 900 ℃ is selected in the step 2), and the holding time is 8 hours, so that the delta phase volume fraction content is ensured to reach 60% -90%.
4. The hot working method for producing the high-uniformity ultra-fine grained nickel-based superalloy according to the claim 1, wherein the heat preservation temperature in the step 3) is 960 ℃, and the heat preservation time is 1 hour, so that the residual volume fraction content of the delta phase is 40-60%.
5. The hot working method for producing the high-uniformity ultra-fine grained nickel-based superalloy as set forth in claim 1, wherein in the steps 1), 2) and 3), the nickel-based superalloy is placed in a heat treatment furnace, timing is started after the temperature is raised to a set temperature and kept for 10min, and the temperature rise rate is not higher than 200 ℃/h.
6. The hot working method for producing a highly homogeneous ultra-fine grained nickel-based superalloy as set forth in claim 1, wherein steps 1), 2) and 3) are performed continuously, and the temperature rise rate is not higher than 200 ℃/h.
7. The hot working method for producing highly homogeneous ultra-fine grained nickel-base superalloy as set forth in claim 1, wherein the step 4) is preferably performed with 1 hot forming, and the total deformation is controlled to be 40%.
8. The hot working method for producing a high-homogeneity ultra-fine grained nickel-based superalloy according to claim 1, wherein the method obtains a nickel-based superalloy with a homogeneous ultra-fine grained structure having a grain size of 8 to 10 grades.
CN202110471311.6A 2021-04-29 2021-04-29 Hot working method for producing high-uniformity ultra-fine grain nickel-based high-temperature alloy Pending CN115261753A (en)

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CN115821180A (en) * 2022-12-06 2023-03-21 浙江浙能技术研究院有限公司 Method for obtaining GH4169 alloy forging with uniform and fine grain structure
CN116200689A (en) * 2023-02-08 2023-06-02 华中科技大学 Pre-forging heat treatment method for nickel-based alloy arc fuse additive prefabricated member

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Publication number Priority date Publication date Assignee Title
CN115821180A (en) * 2022-12-06 2023-03-21 浙江浙能技术研究院有限公司 Method for obtaining GH4169 alloy forging with uniform and fine grain structure
CN116200689A (en) * 2023-02-08 2023-06-02 华中科技大学 Pre-forging heat treatment method for nickel-based alloy arc fuse additive prefabricated member
CN116200689B (en) * 2023-02-08 2024-09-20 华中科技大学 Pre-forging heat treatment method for nickel-based alloy arc fuse additive prefabricated member

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