CN114032481B - Method for homogenizing highly alloyed superalloy materials - Google Patents

Abstract

The invention relates to the technical field of high-temperature alloy hot processing, in particular to a method for homogenizing a high-alloying high-temperature alloy material. The method for homogenizing the high-alloying high-temperature alloy material comprises the following steps: pre-cogging high-alloying high-temperature alloy cast ingots, then carrying out homogenization heat treatment, and then cogging and forging; wherein the pre-cogging treatment comprises: and heating the cast ingot at the temperature of not more than 1200 ℃, and then performing pre-cogging forging. The method of the invention improves the uniformity of the grain structure of the material, in particular the grain structure in the micro-area scale range; the uniformity of the distribution of the second phase in a micro-area scale range is improved, and particularly the size and the area percentage of the primary gamma' phase are more uniform, so that the long-term structure stability and the performance stability are better, and the safety and the reliability of the material in long-term service are higher; the utilization rate and the yield of the material can be improved.

Description

Method for homogenizing highly alloyed superalloy materials

technical field

The invention relates to the technical field of hot processing of superalloys, in particular to a method for homogenizing high-alloyed superalloy materials.

Background technique

Nickel-based deformed superalloys are widely used in the hot-end components of aerospace engines. With the development of advanced aerospace engines, the requirements for the temperature-bearing capacity of superalloy materials are constantly increasing, and more alloying elements are added to the materials. The preparation of highly alloyed superalloys is increasingly difficult, and the segregation of solid solution strengthening elements W, Mo and Cr, as well as elements such as Ti, Nb, and Ta, continues to intensify, and the interdendritic precipitates are more likely to segregate, causing the final material components. The uniformity and the uneven distribution of the second phase bring uncertainty to the performance of the material during long-term service, the microstructure changes irreversibly, and the performance is attenuated.

In recent years, researchers and producers of superalloy materials have improved the degree of segregation of materials by extending the homogenization heat treatment time, or increasing the number of billeting and forging times and the amount of deformation for highly alloyed superalloy materials, but this often increases the Energy consumption, but still can not achieve the purpose of homogenization.

In view of this, the present invention is proposed.

SUMMARY OF THE INVENTION

The purpose of the present invention is to provide a method for homogenizing high-alloying superalloy, so as to solve the technical problems such as micro-segregation of high-alloying superalloy existing in the prior art.

In order to realize the above-mentioned purpose of the present invention, the following technical solutions are specially adopted:

A method for homogenizing a highly alloyed superalloy material, comprising the following steps:

The high-alloyed superalloy ingot is pre-billed, then homogenized and forged;

Wherein, the pre-billing treatment includes: performing pre-billing forging after heating the ingot at a temperature not exceeding 1200°C.

In a specific embodiment of the present invention, the pre-billing treatment includes: performing pre-billing forging after heating the ingot at a temperature not exceeding 1170°C.

In a specific embodiment of the present invention, the pre-blanking process includes:

(a) The temperature is raised to 600-900°C at a rate of ≤120°C/h and kept for more than 4 hours;

(b) heating up to 1100-1150°C at a rate of ≤50°C/h for 4-8 hours;

(c) heating up to 1150-1170°C at a rate of ≤10°C/h for 4-8 hours;

(d) Then, the temperature is lowered to 950-1050°C at a rate of ≤50°C/h and kept for 1-2 hours;

(e) The temperature is then raised to 1100-1170°C at a rate of ≤50°C/h and kept for 1-4 hours before pre-blanking forging.

In the method for homogenizing high-alloyed superalloy materials of the present invention, pre-blanking is performed before the homogenization heat treatment, and a large number of channel defects of element diffusion, such as grain boundaries, phase boundaries, dislocations, etc., are introduced to accelerate the homogenization. The diffusion of elements in the heat treatment process can reduce the time of homogenization heat treatment, save energy, and reduce the segregation index of elements in the material; and then carry out the subsequent blank forging, which solves the problem of the uniformity of the structure of the forging blank prepared by the conventional process. problems such as poor phase uniformity.

In a specific embodiment of the present invention, in the pre-slit forging, the forging times are 1 to 3 times.

In a specific embodiment of the present invention, in the pre-blank forging, the deformation amount per firing is 15% to 45%.

In a specific embodiment of the present invention, the pre-blank forging is performed by means of constrained upsetting.

In a specific embodiment of the present invention, the homogenization heat treatment includes: raising the temperature at a rate of 100-300°C/h to T and holding for ≤12h; then raising the temperature at a rate of 10-30°C/h to 1170-1200°C and holding for 12 hours ~48h; after cooling to below 750°C at a rate of ≤50°C/h, furnace cooling to below 200°C air cooling; where T satisfies: Ts-20°C≤T≤Ts+20°C, Ts is the strengthening phase γ' phase the full melting temperature.

In a specific embodiment of the present invention, the billet forging is performed by means of multi-directional forging.

In a specific embodiment of the present invention, in the billet forging, the forging temperature is 950-1170°C. Further, in the billet forging, the deformation amount per firing is 30% to 60%.

In a specific embodiment of the present invention, the grain size of the pre-blanking-processed blank is grade 2 to 7; the grain size of the forging blank after blanking and forging is grade 8 or finer.

In a specific embodiment of the present invention, the chemical composition of the highly alloyed superalloy in terms of mass percentage includes: C: 0.005%-0.070%, Co: 10%-24%, Cr: 9%-18%, W : 1.0% to 5.0%, Mo: 1.0% to 5.0%, Ti: 1.0% to 6.0%, Al: 0.5% to 4.0%, B: 0.010% to 0.020%, Zr: 0.030% to 0.060%, Nb: 0.5 %～5.0%, Ta: 0%～5%; Fe: ≤1%, the balance is Ni and inevitable impurities.

In a specific embodiment of the present invention, the diameter dimension of the highly alloyed superalloy ingot does not exceed 450 mm. Further, the preparation of the high-alloyed superalloy ingot includes: preparing the electrodes by vacuum induction melting according to alloy components, and then smelting the ingot by electroslag remelting and/or vacuum consumable remelting. Preferably, the ingot is smelted by continuous directional solidification using vacuum induction melting + electroslag remelting.

Compared with the prior art, the beneficial effects of the present invention are:

(1) In the method of the present invention, by adding a certain pre-blanking process, the obtained material has a lower degree of microsegregation, and the segregation indices of typical segregation-prone elements W, Mo, Cr, and Ti are lower;

(2) The method of the present invention improves the uniformity of the grain structure of the material, especially the grain structure in the micro-scale range; improves the uniformity of the second phase distribution in the micro-scale range, especially the primary γ The size and area percentage of the 'phase are more uniform, so that the long-term structure stability and performance stability are better, and the safety and reliability of the material in long-term service are higher; the utilization rate and yield of the material can be improved.

Description of drawings

In order to illustrate the specific embodiments of the present invention or the technical solutions in the prior art more clearly, the following briefly introduces the accompanying drawings that need to be used in the description of the specific embodiments or the prior art. Obviously, the accompanying drawings in the following description The drawings are some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings without creative efforts.

FIG. 1 is a schematic flowchart of a method for homogenizing a highly alloyed superalloy material according to an embodiment of the present invention.

Detailed ways

The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and specific embodiments, but those skilled in the art will understand that the embodiments described below are part of the embodiments of the present invention, rather than all of the embodiments, It is only used to illustrate the present invention and should not be construed as limiting the scope of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention. If the specific conditions are not indicated in the examples, it is carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used without the manufacturer's indication are conventional products that can be purchased from the market.

A method for homogenizing a highly alloyed superalloy material, comprising the following steps:

The high-alloyed superalloy ingot is pre-billed, then homogenized and forged;

Wherein, the pre-billing treatment includes: performing pre-billing forging after heating the ingot at a temperature not exceeding 1200°C.

In a specific embodiment of the present invention, the pre-billing treatment includes: performing pre-billing forging after heating the ingot at a temperature not exceeding 1170°C.

The heating temperature in the pre-blanking treatment is as high as possible within a certain range, and the heating treatment at a temperature not exceeding 1170°C can take into account the energy saving, efficiency improvement and homogenization effect.

The purpose of adopting the above-mentioned pre-blanking treatment in the present invention is mainly to promote the equal re-dissolution of trace boride, η phase or Laves existing between the dendrites of the ingot into the matrix. These precipitates have large size and low melting point, and are easy to become source of crack initiation.

In a specific embodiment of the present invention, the pre-blanking process includes:

(a) The temperature is raised to 600-900°C at a rate of ≤120°C/h and kept for more than 4 hours;

(b) heating up to 1100-1150°C at a rate of ≤50°C/h for 4-8 hours;

(c) heating up to 1150-1170°C at a rate of ≤10°C/h for 4-8 hours;

(d) Then, the temperature is lowered to 950-1050°C at a rate of ≤50°C/h and kept for 1-2 hours;

(e) The temperature is then raised to 1100-1170°C at a rate of ≤50°C/h and kept for 1-4 hours before pre-blanking forging.

As in different embodiments, in the pre-blanking process, the parameters of each step may be as follows, but not limited to this:

In step (a), the heating rate may be 10°C/h, 20°C/h, 30°C/h, 40°C/h, 50°C/h, 60°C/h, 70°C/h, 80°C/h, 90°C/h, 100°C/h, 110°C/h, 120°C/h, etc.; the holding temperature can be 600°C, 650°C, 700°C, 750°C, 800°C, 850°C, 900°C, etc.; The time can further be 4-8h, such as 4h, 5h, 6h, 7h, 8h, etc.;

In step (b), the heating rate can be 10°C/h, 20°C/h, 30°C/h, 40°C/h, 50°C/h, etc.; the holding temperature can be 1100°C, 1110°C, 1120°C, 1130°C, 1140°C, 1150°C, etc.; the holding time can be 4h, 5h, 6h, 7h, 8h, etc.; to dissolve a small amount of low-melting zirconium phase;

In step (c), the heating rate can be 1°C/h, 2°C/h, 3°C/h, 4°C/h, 5°C/h, 6°C/h, 7°C/h, 8°C/h, 9°C/h, 10°C/h, etc.; holding temperature can be 1150°C, 1160°C, 1170°C, etc.; holding time can be 4h, 5h, 6h, 7h, 8h, etc.;

In step (d), the cooling rate can be 10°C/h, 20°C/h, 30°C/h, 40°C/h, 50°C/h, etc.; the holding temperature can be 950°C, 960°C, 970°C, 980°C, 990°C, 1000°C, 1010°C, 1020°C, 1030°C, 1040°C, 1050°C, etc.; holding time can be 1h, 1.5h, 2h, etc.;

In step (e), the heating rate can be 10°C/h, 20°C/h, 30°C/h, 40°C/h, 50°C/h, etc.; the holding temperature can be 1100°C, 1110°C, 1120°C, 1130°C, 1140°C, 1150°C, 1160°C, 1170°C, etc.; the holding time can be 1h, 2h, 3h, 4h, etc.

In the method for homogenizing high-alloyed superalloy materials of the present invention, pre-blanking is performed before the homogenization heat treatment, and a large number of channel defects of element diffusion, such as grain boundaries, phase boundaries, dislocations, etc., are introduced to accelerate the homogenization. The diffusion of elements in the heat treatment process can reduce the time of homogenization heat treatment, save energy, and reduce the segregation index of elements in the material; and then carry out the subsequent blank forging, which solves the problem of the uniformity of the structure of the forging blank prepared by the conventional process. problems such as poor phase uniformity.

In a specific embodiment of the present invention, in the pre-slit forging, the forging times are 1 to 3 times.

In a specific embodiment of the present invention, in the pre-blank forging, the deformation amount per firing is 15% to 45%.

As in different embodiments, in the pre-blank forging, the deformation amount of each fire may be 15%, 20%, 25%, 30%, 35%, 40%, 45% and so on.

In a specific embodiment of the present invention, in the pre-blank forging, the forging times are 3 times. Further, in the pre-blanking forging, the deformation amount of the first fire is 15% to 20%, the deformation amount of the second fire is 25% to 30%, and the deformation amount of the third fire is 40% to 40%. 45%.

The present invention obtains the grain structure in the range of 2-7 grades through the above pre-blanking treatment, increases the area and number of grain boundaries and sub-grain boundaries, and introduces high-density dislocations; The lattice distortion is large, the atomic arrangement is chaotic and loose, the number of vacancies at the grain boundary is large, the energy is high, the diffusion activation energy is smaller than that in the crystal, the atoms are easy to diffuse and migrate, and the high density of dislocation lines is the channel of lattice distortion. , interconnected to form a network, and the diffusion rate of atoms is accelerated; it can make the elements diffuse rapidly in the subsequent homogenization heat treatment process, and the diffusion speed at the grain boundary and subgrain boundary is faster than that in the grain, reducing the time of the homogenization heat treatment, etc., thereby reducing The cost of heat treatment is homogenized, and the grain structure and precipitation phase of the subsequent forging billet can be made more uniform.

In a specific embodiment of the present invention, the pre-blank forging is performed by means of constrained upsetting.

In actual operation, after the pre-blank forging is completed, the blank is subjected to 100% grinding treatment, followed by subsequent homogenization heat treatment and so on.

In a specific embodiment of the present invention, the homogenization heat treatment includes: raising the temperature at a rate of 100-300°C/h to T and holding for ≤12h; then raising the temperature at a rate of 10-30°C/h to 1170-1200°C and holding for 12 hours ~48h; after cooling to below 750°C at a rate of ≤50°C/h, furnace cooling to below 200°C air cooling; where T satisfies: Ts-20°C≤T≤Ts+20°C, Ts is the strengthening phase γ' phase the full melting temperature. Among them, Ts can be measured by metallographic test method.

In different embodiments, in the homogenization heat treatment, the heating rate to T may be 100°C/h, 150°C/h, 200°C/h, 250°C/h, 300°C/h, etc. The time can be ≤6h, such as 1h, 2h, 3h, 4h, 5h, 6h, and so on. In the homogenization heat treatment, the heating rate to 1170-1200°C may be 10°C/h, 15°C/h, 20°C/h, 25°C/h, 30°C/h, etc., and the holding time may be 1170°C. ℃, 1175℃, 1180℃, 1185℃, 1190℃, 1195℃, 1200℃, etc. The holding time can be 12h, 16h, 20h, 24h, 28h, 32h, 36h, 40h, 44h, 48h and so on. In the homogenization heat treatment, the cooling rate to below 750°C may be 10°C/h, 20°C/h, 30°C/h, 40°C/h, 50°C/h, and the like.

Using a heating rate of 100～300℃/h can maintain a high dislocation line density, and at the same time, the number of grain boundaries is the largest in the temperature range of Ts-20℃ to Ts+20℃. At this time, the diffusion of elements is accelerated. The blank can achieve the best element diffusion and homogenization effect under the condition that the heat preservation is not more than 12h. Subsequently, the temperature is raised to 1170-1200°C at a rate of 10-30°C/h and kept for 12-48h to eliminate the segregation of refractory metal elements and the γ-γ' eutectic phase. After the homogenization time exceeds 48h, the elimination of element segregation will basically make no further changes. further improvement.

In a specific embodiment of the present invention, the billet forging is performed by means of multi-directional forging.

In a specific embodiment of the present invention, in the billet forging, the forging temperature is 950-1170°C; preferably, the billet forging has a temperature range of 1000-1170°C. Further, in the billet forging, the deformation amount per firing is 30% to 60%.

In actual operation, in the blank forging, forging can be carried out through multiple fires until a forging blank of the desired shape and size is obtained.

In a specific embodiment of the present invention, the grain size of the pre-blanking-processed blank is grade 2 to 7; the grain size of the forging blank after blanking and forging is grade 8 or finer.

In a specific embodiment of the present invention, the chemical composition of the highly alloyed superalloy in terms of mass percentage includes: C: 0.005%-0.070%, Co: 10%-24%, Cr: 9%-18%, W : 1.0% to 5.0%, Mo: 1.0% to 5.0%, Ti: 1.0% to 6.0%, Al: 0.5% to 4.0%, B: 0.010% to 0.020%, Zr: 0.030% to 0.060%, Nb: 0.5 %～5.0%, Ta: 0%～5%; Fe: ≤1%, the balance is Ni and inevitable impurities. Further, the chemical components in mass percentages include: C: 0.005%-0.070%, Co: 13%-21%, Cr: 13%-16%, W: 2.0%-4.0%, Mo: 3.5%- 4.0%, Ti: 3.0% to 4.0%, Al: 2.0% to 3.5%, B: 0.010% to 0.020%, Zr: 0.030% to 0.060%, Nb: 0.5% to 1.0%, Ta: 0% to 5% ; Fe: ≤ 1%, the remainder is Ni and inevitable impurities. For example, the highly alloyed superalloy may be GH4096, GH4198, but not limited thereto.

By adopting a certain pre-blanking process, the present invention can significantly reduce the micro-segregation degree of the material and the segregation index of the segregation-prone elements for the nickel-based superalloy which is easy to segregate and non-uniform in the conventional process.

In a specific embodiment of the present invention, for the superalloy material subjected to the homogenization treatment, the statistical segregation degree of W is S≤0.25%, the statistical segregation degree of Mo is S≤0.13%, and the statistical segregation degree of Cr is S≤0.038% , Ti statistical segregation degree S≤0.13%.

In a specific embodiment of the present invention, for the superalloy material subjected to the homogenization treatment, the sample standard deviation SD≤1.50 (eg, 0.30-1.05) of the average grain size, and the relative standard deviation RSD≤7.0 of the average grain size % (eg 3.0%～6.5%); the sample standard deviation SD≤0.100 (eg 0.050～0.085) of the average size of the primary γ′ phase, the relative standard deviation RSD≤2.00% (eg 1.50%～2.00) of the average size of the primary γ′ phase %); the sample standard deviation SD≤0.15 (eg 0.05～0.14) of the primary γ′ phase area fraction, the relative standard deviation RSD≤1.50% (eg 0.50%～1.35%) of the primary γ′ phase area fraction; the segregation-prone element W , Mo, Cr, Ti sample standard deviation SD respectively ≤ 0.010 (such as 0.005 ~ 0.008), ≤ 0.010 (such as 0.004 ~ 0.006), ≤ 0.010 (such as 0.004 ~ 0.006), ≤ 0.010 (such as 0.004 ~ 0.006); easy to segregation The relative standard deviation RSD of elements W, Mo, Cr and Ti are respectively ≤0.25% (eg 0.20%～0.22%), ≤0.20% (eg 0.10%～0.13%), ≤0.05% (eg 0.03%～0.04%), ≤0.15% (eg 0.13%～0.14%).

In a specific embodiment of the present invention, the diameter dimension of the highly alloyed superalloy ingot does not exceed 450 mm. Further, the preparation of the high-alloyed superalloy ingot includes: preparing the electrodes by vacuum induction melting according to alloy components, and then smelting the ingot by electroslag remelting and/or vacuum consumable remelting. Preferably, the ingot is smelted by continuous directional solidification using vacuum induction melting + electroslag remelting. Wherein, the preparation process of the ingot can adopt the existing conventional preparation process of the corresponding alloy ingot.

Example 1

This embodiment provides a method for homogenizing GH4096 alloy, referring to Fig. 1, including the following steps:

的GH4096合金铸锭；其中GH4096合金的化学成分按质量百分数计为：C：0.050％，Co：13％，Cr：16％，W：4.0％，Mo：4.0％，Ti：3.80％，Al：2.20％，B：0.015％，Zr：0.050％，Nb：0.70％，余量为Ni及不可避免的杂质。(1) Using vacuum induction melting + electroslag remelting continuous directional solidification to prepare the specifications of

The GH4096 alloy ingot; the chemical composition of the GH4096 alloy by mass percentage is: C: 0.050%, Co: 13%, Cr: 16%, W: 4.0%, Mo: 4.0%, Ti: 3.80%, Al: 2.20%, B: 0.015%, Zr: 0.050%, Nb: 0.70%, and the balance is Ni and inevitable impurities.

(2) the ingot obtained in step (1) is heated to 850°C for 6 hours at 80°C/h, then heated to 1130°C for 6h at 50°C/h, and then heated to 1160°C for 6h at 10°C/h, Then, it was cooled to 1000°C for 1 h at 30°C/h, and then heated to 1150°C at a rate of 50°C/h. The pre-blank forging was carried out for 3 times by means of restrained upsetting. The deformation amount of the first heat was 20%. The deformation amount of the second fire is 30%, the deformation amount of the third fire is 40%, the forging temperature of the last fire is 1100 ℃, and then it is cooled to room temperature for 100% grinding.

(3) Perform high temperature homogenization treatment on the ingot pre-billing treated in step (2), specifically, the temperature is raised at 150°C/h to 1130°C for 6 hours, and then heated to 1190°C at 15°C/h for 24 hours, and then Cool to 750°C at 50°C/h, and then furnace-cool to 200°C for air cooling.

的棒坯。(4) performing billet forging on the ingot after the homogenization treatment in step (3), the forging temperature range is 1000～1170 ℃, a total of 12 firing times, the deformation amount of each firing time is 30%～60%, to obtain

of billets.

Example 2

This embodiment provides a method for homogenizing GH4198 alloy, including the following steps:

的GH4198合金铸锭；其中GH4198合金的化学成分按质量百分数计为：C：0.020％，Co：20.5％，Cr：13％，W：2.3％，Mo：3.8％，Ti：3.80％，Al：3.40％，B：0.015％，Zr：0.050％，Nb：1.0％，Ta：2.5％，余量为Ni及不可避免的杂质。(1) Using vacuum induction melting + electroslag remelting continuous directional solidification to prepare the specifications of

GH4198 alloy ingot; the chemical composition of GH4198 alloy in mass percentage is: C: 0.020%, Co: 20.5%, Cr: 13%, W: 2.3%, Mo: 3.8%, Ti: 3.80%, Al: 3.40%, B: 0.015%, Zr: 0.050%, Nb: 1.0%, Ta: 2.5%, and the balance is Ni and inevitable impurities.

(2) the ingot obtained in step (1) is heated to 850°C for 6 hours at 80°C/h, then heated to 1140°C for 6h at 50°C/h, and then heated to 1170°C for 6h at 10°C/h, Then, it was cooled to 980°C for 1 h at 30°C/h, then heated to 1150°C at a rate of 50°C/h, and pre-blank forging was carried out for 3 times by means of restrained upsetting. The deformation amount of the second fire is 25%, the deformation amount of the third fire is 40%, the forging temperature of the last fire is 1120 ℃, and then cooled to room temperature for 100% grinding.

(3) Perform high temperature homogenization treatment on the ingot pre-billing treated in step (2), specifically, heating the ingot at 160°C/h to 1150°C for 6 hours, then at 15°C/h to 1195°C for 32 hours, and then Cool to 750°C at 50°C/h, and then furnace-cool to 200°C for air cooling.

的棒坯。(4) performing billet forging on the ingot after the homogenization treatment in step (3), the forging temperature range is 1000～1170 ℃, a total of 12 firing times, the deformation amount of each firing time is 30%～50%, to obtain

of billets.

Comparative Example 1

Comparative Example 1 provides a method for the homogenization of conventional GH4096 alloy, including the following steps:

的GH4096合金铸锭；其中GH4096合金的化学成分按质量百分数计为：C：0.050％，Co：13％，Cr：16％，W：4.0％，Mo：4.0％，Ti：3.80％，Al：2.20％，B：0.015％，Zr：0.050％，Nb：0.70％，余量为Ni及不可避免的杂质。(1) Using vacuum induction melting + electroslag remelting continuous directional solidification to prepare the specifications of

The GH4096 alloy ingot; the chemical composition of the GH4096 alloy by mass percentage is: C: 0.050%, Co: 13%, Cr: 16%, W: 4.0%, Mo: 4.0%, Ti: 3.80%, Al: 2.20%, B: 0.015%, Zr: 0.050%, Nb: 0.70%, and the balance is Ni and inevitable impurities.

(2) The ingot obtained in step (1) is subjected to high temperature homogenization treatment. Specifically, the temperature is raised to 850°C for 6 hours at 80°C/h, and then heated to 1130°C for 6 hours at 50°C/h, and then heated to 10°C for 6 hours. /h heat up to 1160°C for 6h, then heat up to 1190°C for 24h at 15°C/h, then cool to 750°C at 50°C/h, then furnace cool to 200°C for air cooling.

的棒坯。(3) carrying out billet forging on the ingot after the homogenization treatment in step (2), the forging temperature range is 1000～1170 ℃, a total of 15 firing times, the deformation amount of each firing time is 30%～60%, to obtain

of billets.

Comparative Example 2

Comparative Example 2 refers to the method of Example 1, and the difference is that the amount of deformation of the pre-blank forging in step (2) is different.

The step (2) of Comparative Example 2 is as follows: the ingot obtained in step (1) is heated to 850°C for 6 hours at 80°C/h, then heated to 1130°C for 6h at 50°C/h, and then heated to 10°C/h for 6 hours. The temperature was raised to 1160°C for 6 hours, then cooled to 1000°C for 1 hour at 30°C/h, and then heated to 1150°C at a rate of 50°C/h. The constrained upsetting method was used for 3 times of blanking and forging, and the deformation amount of the first heat was The deformation amount of the second fire is 10%, the deformation amount of the second fire is 13%, and the deformation amount of the third fire is 15%.

Comparative Example 3

Comparative Example 3 refers to the method of Example 2, and the difference is that the heating rate in step (3) is different.

The step (3) of Comparative Example 3 is: performing high temperature homogenization treatment on the ingot pre-bulleted in step (2), specifically, heating at 70°C/h to 1150°C for 6 hours, and then heating at 15°C/h It was kept at 1195°C for 32h, then cooled to 750°C at 50°C/h, and then furnace cooled to 200°C for air cooling.

Experimental example 1

In order to compare and illustrate the differences in the microstructure of the bar blanks prepared by the methods of different embodiments and comparative examples, the microstructure of any point at the half radius of the cross section of the end of the bar blank is counted, and points are taken every 200 μm spacing, and a total of 6 points, the statistical results of the average grain size (500 magnification field of view) are shown in Table 1, the average size of the primary γ' phase (500 magnification field of view) is shown in Table 2, and the primary γ' phase area fraction (500 magnification field of view) is shown in Table 2 3. The microstructure of any point at the half radius of the cross section at the end of the billet was counted, and points were taken at intervals of 100 μm, and a total of 10 points were taken. Electron probes were used to detect the contents of elements W, Mo, Cr, and Ti in Table 4.

Table 1 Average grain size (μm)

Location 1 o'clock 2:00 3 points 4 o'clock 5 o'clock 6 o'clock Example 1 12 12.5 13 12.5 12.2 12 Example 2 15 15.5 16 16.5 16.5 18 Comparative Example 1 10 15 20 12 11 10 Comparative Example 2 9 11 13 12 15 17 Comparative Example 3 14 15.5 16 15 18 19

Table 2 Average size of primary γ' phase (μm)

Table 3 Primary γ' phase area fraction (%)

Location 1 o'clock 2:00 3 points 4 o'clock 5 o'clock 6 o'clock Example 1 9.5 9.6 9.5 9.6 9.5 9.5 Example 2 10 10.2 10.3 10 10 10.2 Comparative Example 1 9.7 9.0 8.0 9.6 9.5 9.7 Comparative Example 2 9.0 9.5 9.4 9.6 9.2 9.6 Comparative Example 3 9.8 10.3 10.4 10.0 9.9 10.4

Table 4 Elements W, Mo, Cr, Ti content (wt%)

Remarks: Take statistical segregation degree S as the criterion of segregation index, S=(c ₂ -c ₁ )/2c ₀ , where c ₂ is the upper limit of the statistical range, c ₁ is the lower limit of the statistical range, and c ₀ is the content mean

It can be seen from the above test results that the GH4096 alloy billet in Example 1 of the present invention has a grain size range of 12 to 13 μm in different micro-domains, an average size of the primary γ′ phase in the range of 3.5 to 3.6 μm, and the area of the primary γ′ phase is in the range of 12 to 13 μm. The fractions range from 9.5% to 9.6%, and the content deviation of typical elements in different microdomains is small. For the GH4198 alloy billet in Example 2 of the present invention, the grain size of different micro-regions ranges from 15 to 18 μm, the average size of the primary γ’ phase ranges from 4.1 to 4.3 μm, and the area fraction of the primary γ’ phase ranges from 10% to 10%. 10.3%, the content deviation of typical elements in different microdomains is very small. In the GH4096 alloy billet of Comparative Example 1, the grain size of different micro-regions ranges from 10 to 20 μm, and the grain size deviation is large; the average size of the primary γ′ phase ranges from 3.0 to 3.8 μm; The fraction ranges from 8.0% to 9.7%, and the primary γ' phase distribution is not uniform; the content deviation of typical elements in different micro-regions is large. Similarly, for the GH4096 bar blank in Comparative Example 2, the segregation degrees of typical segregation-prone elements in different microregions are larger than those in Example 1, but smaller than those in Comparative Example 1; for the GH4198 bar blank in Comparative Example 3, the The typical element segregation degree is larger than that of Example 2. The method of the present invention is further described, which improves the uniformity of the grain structure of the material, especially the grain structure in the micro-scale range; improves the uniformity of the second phase distribution in the micro-scale range, especially the primary γ The size and area percentage of the 'phase are more uniform, so that the long-term structure stability and performance stability are better, and the safety and reliability of the material in long-term service are higher; the utilization rate and yield of the material can be improved.

Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, but not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: The technical solutions described in the foregoing embodiments can still be modified, or some or all of the technical features thereof can be equivalently replaced; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the technical solutions of the embodiments of the present invention. scope.

Claims (9)

1. the method for homogenizing high-alloyed superalloy material, is characterized in that, comprises the steps: The high-alloyed superalloy ingots are pre-billed, then homogenized and forged; Wherein, the pre-billing treatment includes: pre-billing forging after heating the ingot at a temperature not exceeding 1170°C; The pre-blanking process includes: (a) The temperature is raised to 600~900°C at a rate of ≤120°C/h and kept for more than 4 hours; (b) Heat the temperature to 1100~1150°C at a rate of ≤50°C/h for 4~8h; (c) Heat the temperature to 1150~1170°C at a rate of ≤10°C/h for 4~8h; (d) Then cool down to 950~1050°C at a rate of ≤50°C/h for 1~2h; (e) Heat up to 1100~1170°C at a rate of ≤50°C/h for 1~4h and then pre-blank forging; The homogenization heat treatment includes: raising the temperature at a rate of 100-300°C/h to T for ≤12h; then raising the temperature at a rate of 10-30°C/h to 1170-1200°C for 12-48h; and then heating at a rate of ≤50°C/h After cooling at a rate of h below 750°C, furnace cooling to below 200°C air cooling; where T satisfies: Ts-20°C≤T≤Ts+20°C, Ts is the total dissolution temperature of the strengthening phase γ´ phase; The grain size of the pre-blanking-processed billet is 2-7 grades; the grain size of the forging blanks after blanking and forging is 8-grade or finer; The chemical composition of the high-alloying superalloy in terms of mass percentage includes: C: 0.005%-0.070%, Co: 10%-24%, Cr: 9%-18%, W: 1.0%-5.0%, Mo: 1.0%~5.0%, Ti: 1.0%~6.0%, Al: 0.5%~4.0%, B: 0.010%~0.020%, Zr: 0.030%~0.060%, Nb: 0.5%~5.0%, Ta: 0% ~5%; Fe: ≤1%, the balance is Ni and inevitable impurities. 2 . The method for homogenizing a highly alloyed superalloy material according to claim 1 , wherein, in the pre-billing forging, the forging times are 1 to 3 times. 3 . 3. The method for homogenizing high-alloyed superalloy material according to claim 2, characterized in that, in the pre-billing forging, the amount of deformation per firing is 15% to 45%. 4 . The method for homogenizing a highly alloyed superalloy material according to claim 1 , wherein the pre-blank forging is performed by means of constrained upsetting. 5 . 5 . The method for homogenizing a highly alloyed superalloy material according to claim 1 , wherein the billet forging is performed by means of multi-directional forging. 6 . 6 . The method for homogenizing a highly alloyed superalloy material according to claim 1 , wherein, in the billet forging, the forging temperature is 950-1170° C. 7 . 7. The method for homogenizing high-alloyed superalloy material according to claim 1, characterized in that, in the billet forging, the amount of deformation per firing is 30% to 60%. 8 . The method for homogenizing a highly alloyed superalloy material according to claim 1 , wherein the diameter dimension of the highly alloyed superalloy ingot is not more than 450 mm. 9 . 9. The method for homogenizing high-alloyed superalloy material according to claim 1, wherein the preparation of the high-alloyed superalloy ingot comprises: preparing electrodes by vacuum induction melting according to alloy ingredients, The ingot is subsequently smelted using electroslag remelting and/or vacuum consumable remelting.

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