CN114032481B - Method for homogenizing high-alloying high-temperature alloy material - Google Patents
Method for homogenizing high-alloying high-temperature alloy material Download PDFInfo
- Publication number
- CN114032481B CN114032481B CN202111386023.7A CN202111386023A CN114032481B CN 114032481 B CN114032481 B CN 114032481B CN 202111386023 A CN202111386023 A CN 202111386023A CN 114032481 B CN114032481 B CN 114032481B
- Authority
- CN
- China
- Prior art keywords
- cogging
- forging
- temperature
- equal
- homogenizing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J1/00—Preparing metal stock or similar ancillary operations prior, during or post forging, e.g. heating or cooling
- B21J1/06—Heating or cooling methods or arrangements specially adapted for performing forging or pressing operations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/002—Hybrid process, e.g. forging following casting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/06—Methods for forging, hammering, or pressing; Special equipment or accessories therefor for performing particular operations
- B21J5/08—Upsetting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Forging (AREA)
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
Technical Field
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.
Background
The nickel-based wrought superalloy is widely applied to hot end parts of aerospace engines, and with the development of advanced aerospace engines, the requirement on the temperature bearing capacity of a superalloy material is continuously improved, and more alloying elements are added into the material. The preparation difficulty of high-alloying high-temperature alloy is increased continuously, segregation of solid solution strengthening elements W, Mo and Cr, Ti, Nb, Ta and the like is increased continuously, a precipitated phase among dendrites is easier to be deviated, the structural tissue of a final material member is not uniform, the distribution of a second phase is not uniform, uncertainty is brought to the performance of the material in the long-term service process, the microstructure is irreversibly changed, the performance is attenuated and the like.
In recent years, high-temperature alloy material researches and manufacturers aim at high-alloying high-temperature alloy materials, the segregation degree of the materials is improved by means of prolonging homogenization heat treatment time, increasing cogging and forging heat number and deformation, and the like, but the energy consumption is increased, but the homogenization purpose is still not achieved.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a method for homogenizing high-alloying high-temperature alloy so as to solve the technical problems of microsegregation and the like of the high-alloying high-temperature alloy in the prior art.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
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.
In a particular embodiment of the invention, the pre-cogging treatment comprises: and heating the cast ingot at a temperature not exceeding 1170 ℃, and then performing pre-cogging forging.
In a particular embodiment of the invention, the pre-cogging treatment comprises:
(a) heating to 600-900 ℃ at the speed of less than or equal to 120 ℃/h, and preserving the heat for more than 4 h;
(b) heating to 1100-1150 ℃ at the speed of less than or equal to 50 ℃/h, and preserving the heat for 4-8 h;
(c) then raising the temperature to 1150-1170 ℃ at the speed of less than or equal to 10 ℃/h and preserving the temperature for 4-8 h;
(d) then cooling to 950-1050 ℃ at the speed of less than or equal to 50 ℃/h, and preserving heat for 1-2 h;
(e) then raising the temperature to 1100-1170 ℃ at the speed of less than or equal to 50 ℃/h, and preserving the temperature for 1-4 h, and then performing pre-cogging forging.
According to the method for homogenizing the high-alloying high-temperature alloy material, pre-cogging is carried out before homogenization heat treatment, and channel defects of large-amount element diffusion, such as crystal boundaries, phase boundaries, dislocation and the like, are introduced, so that the diffusion of elements in the homogenization heat treatment process is accelerated, the time of the homogenization heat treatment can be shortened, the energy is saved, and the segregation index of the elements in the material is reduced; and subsequent cogging forging is carried out, so that the problems of poor structure uniformity and second phase uniformity of the forged blank prepared by the conventional process and the like are solved.
In a specific embodiment of the present invention, in the pre-cogging forging, the number of forging shots is 1 to 3.
In a specific embodiment of the present invention, the amount of deformation per one firing in the pre-cogging forging is 15% to 45%.
In a particular embodiment of the invention, the pre-cogging forging is performed in a restrained-upset manner.
In a particular embodiment of the invention, the homogenization heat treatment comprises: heating at the speed of 100-300 ℃/h until the temperature T is less than or equal to 12 h; heating to 1170-1200 ℃ at the speed of 10-30 ℃/h, and keeping the temperature for 12-48 h; cooling to below 750 ℃ at a speed of less than or equal to 50 ℃/h, and then cooling in a furnace to below 200 ℃ for air cooling; wherein T satisfies: t is more than or equal to Ts-20 ℃ and less than or equal to Ts +20 ℃, and Ts is the total dissolution temperature of the reinforcing phase gamma'.
In a specific embodiment of the present invention, the cogging forging is performed by a multidirectional forging method.
In a specific embodiment of the present invention, the forging temperature in the cogging forging is 950 to 1170 ℃. Further, in the cogging forging, the deformation amount per firing is 30 to 60 percent.
In a specific embodiment of the invention, the grain size of the pre-cogging processed blank is 2-7 grades; the grain size of the forging stock after cogging forging is grade 8 or finer.
In a specific embodiment of the present invention, the chemical composition of the high alloying superalloy comprises, in mass percent: 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 to 0.060%, Nb: 0.5% -5.0%, Ta: 0% -5%; fe: less than or equal to 1 percent, and the balance of Ni and inevitable impurities.
In a particular embodiment of the invention, the high alloying superalloy ingot has a diameter dimension of no more than 450 mm. Further, the preparation of the high-alloying high-temperature alloy ingot comprises the following steps: preparing materials according to alloy components, preparing an electrode by adopting vacuum induction melting, and then smelting an ingot by adopting electroslag remelting and/or vacuum consumable remelting. Preferably, the ingot is smelted by adopting vacuum induction smelting and electroslag remelting continuous directional solidification.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the method, a certain pre-cogging procedure is added, so that the obtained material is lower in microsegregation degree, and the segregation indexes of typical easy-segregation elements W, Mo, Cr and Ti are lower;
(2) 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.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic flow chart of a method for homogenizing a high-alloying superalloy material according to an embodiment of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
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.
In a particular embodiment of the invention, said pre-cogging treatment comprises: and heating the cast ingot at a temperature not exceeding 1170 ℃, and then performing pre-cogging forging.
The higher the heating temperature in the pre-cogging treatment is in a certain range, the better the heating temperature is, the heating treatment is carried out at the temperature not exceeding 1170 ℃, and the energy conservation, the efficiency improvement and the homogenization effect can be ensured at the same time.
The purpose of the pre-cogging treatment adopted by the invention is mainly to promote micro boride, eta phase or Laves phase existing among ingot dendrites to be equally dissolved back into a matrix, and the precipitated phases have large size and low melting point and are easy to become crack initiation sources in the forging process.
In a particular embodiment of the invention, the pre-cogging treatment comprises:
(a) heating to 600-900 ℃ at the speed of less than or equal to 120 ℃/h, and preserving the heat for more than 4 h;
(b) heating to 1100-1150 ℃ at the speed of less than or equal to 50 ℃/h, and preserving the heat for 4-8 h;
(c) then raising the temperature to 1150-1170 ℃ at the speed of less than or equal to 10 ℃/h and preserving the temperature for 4-8 h;
(d) then cooling to 950-1050 ℃ at the speed of less than or equal to 50 ℃/h, and preserving heat for 1-2 h;
(e) then raising the temperature to 1100-1170 ℃ at the speed of less than or equal to 50 ℃/h, and preserving the temperature for 1-4 h, and then performing pre-cogging forging.
In the pre-blooming process, as in different embodiments, the respective step parameters may be as follows, but are not limited to the following:
in the step (a), the heating rate can be 10 ℃/h, 20 ℃/h, 30 ℃/h, 40 ℃/h, 50 ℃/h, 60 ℃/h, 70 ℃/h, 80 ℃/h, 90 ℃/h, 100 ℃/h, 110 ℃/h, 120 ℃/h and the like; the temperature can be 600 deg.C, 650 deg.C, 700 deg.C, 750 deg.C, 800 deg.C, 850 deg.C, 900 deg.C, etc.; the heat preservation time can be further 4-8 h, such as 4h, 5h, 6h, 7h, 8h and the like;
in the step (b), the heating rate can be 10 ℃/h, 20 ℃/h, 30 ℃/h, 40 ℃/h, 50 ℃/h and the like; the temperature can be 1100 deg.C, 1110 deg.C, 1120 deg.C, 1130 deg.C, 1140 deg.C, 1150 deg.C, etc.; the heat preservation time can be 4h, 5h, 6h, 7h, 8h and the like; to dissolve trace amounts of low melting zirconium compound phases;
in the step (c), the heating rate can be 1 ℃/h, 2 ℃/h, 3 ℃/h, 4 ℃/h, 5 ℃/h, 6 ℃/h, 7 ℃/h, 8 ℃/h, 9 ℃/h, 10 ℃/h and the like; the temperature can be 1150 ℃, 1160 ℃, 1170 ℃ and the like; the heat preservation time can be 4h, 5h, 6h, 7h, 8h and the like;
in the step (d), the cooling rate can be 10 ℃/h, 20 ℃/h, 30 ℃/h, 40 ℃/h, 50 ℃/h and the like; the temperature can be 950 deg.C, 960 deg.C, 970 deg.C, 980 deg.C, 990 deg.C, 1000 deg.C, 1010 deg.C, 1020 deg.C, 1030 deg.C, 1040 deg.C, 1050 deg.C, etc.; the heat preservation time can be 1h, 1.5h, 2h and the like;
in the step (e), the heating rate can be 10 ℃/h, 20 ℃/h, 30 ℃/h, 40 ℃/h, 50 ℃/h and the like; the temperature can be 1100 deg.C, 1110 deg.C, 1120 deg.C, 1130 deg.C, 1140 deg.C, 1150 deg.C, 1160 deg.C, 1170 deg.C, etc.; the holding time can be 1h, 2h, 3h, 4h, and the like.
According to the method for homogenizing the high-alloying high-temperature alloy material, pre-cogging is carried out before homogenization heat treatment, and channel defects of large-amount element diffusion, such as crystal boundaries, phase boundaries, dislocation and the like, are introduced, so that the diffusion of elements in the homogenization heat treatment process is accelerated, the time of the homogenization heat treatment can be shortened, the energy is saved, and the segregation index of the elements in the material is reduced; and subsequent cogging forging is carried out, so that the problems of poor structure uniformity and second phase uniformity of the forged blank prepared by the conventional process and the like are solved.
In a specific embodiment of the present invention, in the pre-cogging forging, the number of forging shots is 1 to 3.
In a specific embodiment of the present invention, the amount of deformation per one firing in the pre-cogging forging is 15% to 45%.
As in the different embodiments, the amount of deformation per fire in the pre-cogging forging may be 15%, 20%, 25%, 30%, 35%, 40%, 45%, etc.
In a specific embodiment of the present invention, in the pre-cogging forging, the number of forging passes is 3. Furthermore, in the pre-cogging forging, the deformation amount of the first heating is 15-20%, the deformation amount of the second heating is 25-30%, and the deformation amount of the third heating is 40-45%.
According to the invention, by the pre-cogging treatment, a grain structure in a 2-7 level range is obtained, the area and the number of grain boundaries and subgrain boundaries are increased, and high-density dislocation is introduced; because the lattice distortion at the crystal boundary and the subcrystal boundary is larger, the atomic arrangement is disordered and loose, the number of vacancies at the crystal boundary is larger, the energy is higher, the diffusion activation energy is smaller than that in the crystal, the atoms are easy to diffuse and move, and the high-density dislocation lines are pipelines with lattice distortion and are communicated with each other to form a network, so that the diffusion speed of the atoms is accelerated; the method can quickly diffuse elements in the subsequent homogenization heat treatment process, has higher diffusion speed in a crystal boundary and a subgrain boundary, reduces the time of homogenization heat treatment, and the like, further reduces the cost of the homogenization heat treatment, and can make the grain structure and the precipitated phase of the subsequent forging stock more uniform.
In a particular embodiment of the invention, the pre-cogging forging is performed in a restrained-upset manner.
In actual operation, after pre-cogging forging is completed, the blank is subjected to 100% polishing treatment, and then subsequent homogenization heat treatment and the like.
In a particular embodiment of the invention, the homogenization heat treatment comprises: heating at the speed of 100-300 ℃/h until the temperature T is less than or equal to 12 h; heating to 1170-1200 ℃ at the speed of 10-30 ℃/h, and keeping the temperature for 12-48 h; cooling to below 750 ℃ at a speed of less than or equal to 50 ℃/h, and then cooling in a furnace to below 200 ℃ for air cooling; wherein T satisfies: t is more than or equal to Ts-20 ℃ and less than or equal to Ts +20 ℃, and Ts is the total dissolution temperature of the reinforcing phase gamma'. Wherein Ts can be measured by a metallographic test method.
In the homogenizing heat treatment, the heating rate of heating to T can be 100 ℃/h, 150 ℃/h, 200 ℃/h, 250 ℃/h, 300 ℃/h and the like, and the holding time can be less than or equal to 6h, such as 1h, 2h, 3h, 4h, 5h, 6h and the like. In the homogenization heat treatment, the heating rate of heating to 1170-1200 ℃ can be 10 ℃/h, 15 ℃/h, 20 ℃/h, 25 ℃/h, 30 ℃/h and the like, the heat preservation time can be 1170 ℃, 1175 ℃, 1180 ℃, 1185 ℃, 1190 ℃, 1195 ℃, 1200 ℃ and the like, and the heat preservation time can be 12h, 16h, 20h, 24h, 28h, 32h, 36h, 40h, 44h, 48h and the like. In the homogenization heat treatment, the cooling rate of cooling to below 750 ℃ can be 10 ℃/h, 20 ℃/h, 30 ℃/h, 40 ℃/h, 50 ℃/h and the like.
The heating rate of 100-300 ℃/h is adopted to keep higher dislocation linear density, and the number of crystal boundaries is the largest in the temperature range of Ts-20 ℃ to Ts +20 ℃, so that the element diffusion is accelerated, and the best element diffusion homogenization effect can be achieved under the condition that the temperature is not more than 12h by matching with the pre-cogging. And then heating to 1170-1200 ℃ at the speed of 10-30 ℃/h, and preserving the temperature for 12-48 h to eliminate the refractory metal element segregation and the gamma-gamma' eutectic phase, wherein the elimination of the element segregation is basically not further improved after the homogenization time exceeds 48 h.
In a specific embodiment of the present invention, the cogging forging is performed by a multidirectional forging method.
In a specific embodiment of the invention, in the cogging forging, the forging temperature is 950-1170 ℃; preferably, the temperature range of the cogging forging is 1000-1170 ℃. Further, in the cogging forging, the deformation amount per firing is 30 to 60 percent.
In practice, the cogging forging may be performed by multiple passes until a billet of the desired shape and size is obtained.
In a specific embodiment of the invention, the grain size of the pre-cogging processed blank is 2-7 grades; the grain size of the forging stock after cogging forging is grade 8 or finer.
In a specific embodiment of the present invention, the chemical composition of the high alloying superalloy comprises, in mass percent: 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 to 0.060%, Nb: 0.5% -5.0%, Ta: 0% -5%; fe: less than or equal to 1 percent, and the balance of Ni and inevitable impurities. Further, the chemical components comprise the following components in percentage by mass: c: 0.005% -0.070%, Co: 13% -21%, Cr: 13% -16%, W: 2.0% -4.0%, Mo: 3.5% -4.0%, Ti: 3.0% -4.0%, Al: 2.0% -3.5%, B: 0.010-0.020%, Zr: 0.030 to 0.060%, Nb: 0.5% -1.0%, Ta: 0% -5%; fe: less than or equal to 1 percent, and the balance of Ni and inevitable impurities. For example, the high-alloying high-temperature alloy can be GH4096 or GH4198, but is not limited thereto.
By adopting a certain pre-cogging procedure, the invention can obviously reduce the micro-segregation degree of the material and reduce the segregation index of the segregation-prone element aiming at the nickel-based high-temperature alloy which is easy to segregate and uneven in the conventional process.
In a specific embodiment of the invention, the statistical segregation degree S of W is less than or equal to 0.25%, the statistical segregation degree S of Mo is less than or equal to 0.13%, the statistical segregation degree S of Cr is less than or equal to 0.038%, and the statistical segregation degree S of Ti is less than or equal to 0.13% in the homogenized high-temperature alloy material.
In a specific embodiment of the invention, the sample standard deviation SD of the average grain size is less than or equal to 1.50 (such as 0.30-1.05) and the relative standard deviation RSD of the average grain size is less than or equal to 7.0 (such as 3.0-6.5 percent) through the homogenized high-temperature alloy material; the standard deviation SD of the sample of the average size of the primary gamma 'phase is less than or equal to 0.100 (such as 0.050-0.085), and the relative standard deviation RSD of the average size of the primary gamma' phase is less than or equal to 2.00 percent (such as 1.50-2.00 percent); the standard deviation SD of the sample of the primary gamma 'phase area fraction is less than or equal to 0.15 (such as 0.05-0.14), and the relative standard deviation RSD of the primary gamma' phase area fraction is less than or equal to 1.50 (such as 0.50-1.35%); the standard deviation SD of the easy segregation elements W, Mo, Cr and Ti is respectively less than or equal to 0.010 (such as 0.005-0.008), less than or equal to 0.010 (such as 0.004-0.006) and less than or equal to 0.010 (such as 0.004-0.006); the relative standard deviation RSD of the segregation-prone elements W, Mo, Cr and Ti is respectively less than or equal to 0.25 percent (such as 0.20 to 0.22 percent), less than or equal to 0.20 percent (such as 0.10 to 0.13 percent), less than or equal to 0.05 percent (such as 0.03 to 0.04 percent) and less than or equal to 0.15 percent (such as 0.13 to 0.14 percent).
In a particular embodiment of the invention, the high alloying superalloy ingot has a diameter dimension of no more than 450 mm. Further, the preparation of the high-alloying high-temperature alloy ingot comprises the following steps: preparing materials according to alloy components, preparing an electrode by adopting vacuum induction melting, and then smelting an ingot by adopting electroslag remelting and/or vacuum consumable remelting. Preferably, the ingot is smelted by adopting vacuum induction smelting and electroslag remelting continuous directional solidification. The preparation process of the cast ingot can adopt the conventional preparation process of the corresponding alloy cast ingot.
Example 1
This example provides a method for homogenizing GH4096 alloys, with reference to fig. 1, comprising the following steps:
(1) the vacuum induction melting and electroslag remelting continuous directional solidification preparation method is adopted to obtain the alloy with the specification of
GH4096 alloy ingot casting; the GH4096 alloy comprises the following chemical components in percentage by mass: c: 0.050%, Co: 13%, Cr: 16%, W: 4.0%, Mo: 4.0%, Ti: 3.80%, Al: 2.20%, B: 0.015%, Zr: 0.050Percent, Nb: 0.70%, and the balance of Ni and inevitable impurities.
(2) Heating the ingot obtained in the step (1) to 850 ℃ at a speed of 80 ℃/h, preserving heat for 6h, heating to 1130 ℃ at a speed of 50 ℃/h, preserving heat for 6h, heating to 1160 ℃ at a speed of 10 ℃/h, preserving heat for 6h, cooling to 1000 ℃ at a speed of 30 ℃/h, preserving heat for 1h, heating to 1150 ℃ at a speed of 50 ℃/h, pre-cogging and forging for 3 times by adopting a constraint upsetting mode, wherein the deformation of the first time is 20%, the deformation of the second time is 30%, the deformation of the third time is 40%, the forging temperature of the last time is 1100 ℃, cooling to room temperature, and polishing by 100%.
(3) And (3) carrying out high-temperature homogenization treatment on the ingot subjected to the pre-cogging treatment in the step (2), specifically, heating to 1130 ℃ at the speed of 150 ℃/h, preserving heat for 6h, then heating to 1190 ℃ at the speed of 15 ℃/h, preserving heat for 24h, then cooling to 750 ℃ at the speed of 50 ℃/h, and then cooling to 200 ℃ in a furnace, and discharging and air cooling.
(4) Cogging and forging the cast ingot after homogenization treatment in the step (3), wherein the forging temperature range is 1000-1170 ℃, the total number of firing is 12, and the deformation per firing is 30-60%, so as to obtain the cast ingot
The rod blank of (1).
Example 2
This example provides a method of GH4198 alloy homogenization comprising the steps of:
(1) the vacuum induction melting and electroslag remelting continuous directional solidification preparation method is adopted to obtain the alloy with the specification of
GH4198 alloy ingot of (a); the GH4198 alloy comprises the following chemical components in percentage by mass: 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 of Ni and inevitable impurities.
(2) Heating the ingot obtained in the step (1) to 850 ℃ at a speed of 80 ℃/h, preserving heat for 6h, heating to 1140 ℃ at a speed of 50 ℃/h, preserving heat for 6h, heating to 1170 ℃ at a speed of 10 ℃/h, preserving heat for 6h, cooling to 980 ℃ at a speed of 30 ℃/h, preserving heat for 1h, heating to 1150 ℃ at a speed of 50 ℃/h, pre-cogging and forging for 3 fire times in a constrained upsetting mode, wherein the deformation of the first fire time is 20%, the deformation of the second fire time is 25%, the deformation of the third fire time is 40%, and the forging temperature of the first fire is 1120 ℃, cooling to room temperature, and polishing for 100%.
(3) And (3) carrying out high-temperature homogenization treatment on the ingot subjected to the pre-cogging treatment in the step (2), specifically, heating to 1150 ℃ at 160 ℃/h, preserving heat for 6h, then heating to 1195 ℃ at 15 ℃/h, preserving heat for 32h, then cooling to 750 ℃ at 50 ℃/h, and then cooling to 200 ℃ in a furnace, and discharging and air cooling.
(4) Cogging and forging the cast ingot after homogenization treatment in the step (3), wherein the forging temperature range is 1000-1170 ℃, the total number of firing times is 12, and the deformation per firing time is 30-50%, so as to obtain the cast ingot
The rod blank of (1).
Comparative example 1
Comparative example 1 provides a method of homogenization of a conventional GH4096 alloy comprising the steps of:
(1) the vacuum induction melting and electroslag remelting continuous directional solidification preparation method is adopted to obtain the alloy with the specification of
GH4096 alloy ingot casting; the GH4096 alloy comprises the following chemical components in percentage by mass: 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 of Ni and inevitable impurities.
(2) And (2) carrying out high-temperature homogenization treatment on the ingot obtained in the step (1), specifically, heating to 850 ℃ at a speed of 80 ℃/h, keeping the temperature for 6h, heating to 1130 ℃ at a speed of 50 ℃/h, keeping the temperature for 6h, heating to 1160 ℃ at a speed of 10 ℃/h, keeping the temperature for 6h, heating to 1190 ℃ at a speed of 15 ℃/h, keeping the temperature for 24h, cooling to 750 ℃ at a speed of 50 ℃/h, cooling to 200 ℃ in a furnace, and taking out the ingot from the furnace for air cooling.
(3) Cogging and forging the cast ingot after the homogenization treatment in the step (2), wherein the forging temperature range is 1000-1170 ℃,15 times of fire in total, and the deformation of each fire is 30 to 60 percent to obtain the product
The rod blank of (1).
Comparative example 2
Comparative example 2 the process of example 1 was referenced, with the following differences: and (3) the deformation of the pre-cogging forging in the step (2) is different.
Step (2) of comparative example 2 was: heating the ingot obtained in the step (1) to 850 ℃ at a speed of 80 ℃/h, preserving heat for 6h, heating to 1130 ℃ at a speed of 50 ℃/h, preserving heat for 6h, heating to 1160 ℃ at a speed of 10 ℃/h, preserving heat for 6h, cooling to 1000 ℃ at a speed of 30 ℃/h, preserving heat for 1h, heating to 1150 ℃ at a speed of 50 ℃/h, forging for 3 times by adopting a constrained upsetting mode, wherein the first-time deformation is 10%, the second-time deformation is 13%, the third-time deformation is 15%, the last-time forging temperature is 1100 ℃, cooling to room temperature, and polishing by 100%.
Comparative example 3
Comparative example 3 the process of example 2 was referenced, with the following differences: the heating rates in step (3) are different.
Step (3) of comparative example 3 was: and (3) carrying out high-temperature homogenization treatment on the ingot subjected to the pre-cogging treatment in the step (2), specifically, heating to 1150 ℃ at a speed of 70 ℃/h, preserving heat for 6h, then heating to 1195 ℃ at a speed of 15 ℃/h, preserving heat for 32h, then cooling to 750 ℃ at a speed of 50 ℃/h, and then cooling to 200 ℃ in a furnace, and discharging and air cooling.
Experimental example 1
In order to illustrate the differences of the microstructures and the like of the bar stocks prepared by the methods of different examples and comparative examples, the microstructures of any point at one half radius of the cross section of the end part of the bar stock are counted, the points are taken at intervals of 200 μm and are totally 6 points, the statistical result of the average grain size (500 multiplying power visual field) is shown in table 1, the average size (500 multiplying power visual field) of the primary gamma 'phase is shown in table 2, and the area fraction (500 multiplying power visual field) of the primary gamma' phase is shown in table 3. Counting the microstructure of any point at one half radius of the cross section of the end of the bar billet, taking 10 points at intervals of 100 mu m, and detecting the contents of elements W, Mo, Cr and Ti by using an electronic probe as shown in Table 4.
TABLE 1 average grain size (. mu.m)
| Position of | 1 point | 2 point | 3 point | 4 points | 5 point | 6 points |
| 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 Primary gamma' phase mean size (. mu.m)
TABLE 3 Primary gamma prime area fraction (%)
| Position of | 1 point | 2 point | 3 point | 4 points | 5 point | 6 points |
| 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 contents (wt%) of W, Mo, Cr, and Ti elements
Remarking: taking statistical segregation degree S as criterion of segregation index, S ═ c2-c1)/2c0Wherein c is2Is the upper limit of the statistical range, c1As the lower limit of the statistical range, c0Is the content average value
From the test results, the GH4096 alloy bar billet of example 1 of the present invention has a grain size range of 12 to 13 μm in different micro-regions, an average size range of primary γ 'phase of 3.5 to 3.6 μm, an area fraction range of primary γ' phase of 9.5 to 9.6%, and a small content deviation of typical elements in different micro-regions. In the GH4198 alloy bar blank of the embodiment 2, the grain sizes of different micro areas are within 15-18 mu m, the average size range of primary gamma 'phase is 4.1-4.3 mu m, the area fraction range of the primary gamma' phase is 10-10.3%, and the content deviation of typical elements of different micro areas is very small. The GH4096 alloy bar blank of the comparative example 1 has the grain sizes of different micro areas within the range of 10-20 μm, and has larger grain size deviation; the average size range of the primary gamma' phase is 3.0-3.8 mu m; the area fraction range of the primary gamma phase is 8.0-9.7%, and the primary gamma phase is not uniformly distributed; the content deviation of typical elements of different micro-regions is large. Similarly, in the GH4096 bar of comparative example 2, the segregation degree of typical segregation-prone elements in different micro-regions is greater than that of example 1, but smaller than that of comparative example 1; the GH4198 bar of comparative example 3 had a higher degree of segregation of typical elements in different domains than that of example 2. Further illustrating the method of the present invention, the grain structure uniformity of the material is improved, especially 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 yield of the material can be improved.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. The method for homogenizing the high-alloying high-temperature alloy material is characterized by comprising the following steps of:
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: heating the cast ingot at a temperature not exceeding 1170 ℃, and then performing pre-cogging forging;
the pre-cogging treatment comprises the following steps:
(a) heating to 600-900 ℃ at the speed of less than or equal to 120 ℃/h, and preserving the heat for more than 4 h;
(b) heating to 1100-1150 ℃ at the speed of less than or equal to 50 ℃/h, and preserving the heat for 4-8 h;
(c) then raising the temperature to 1150-1170 ℃ at the speed of less than or equal to 10 ℃/h and preserving the temperature for 4-8 h;
(d) then cooling to 950-1050 ℃ at the speed of less than or equal to 50 ℃/h, and preserving heat for 1-2 h;
(e) heating to 1100-1170 ℃ at the speed of less than or equal to 50 ℃/h, and preserving heat for 1-4 h, and then performing pre-cogging forging;
the homogenizing heat treatment comprises: heating at the speed of 100-300 ℃/h until the temperature T is less than or equal to 12 h; heating to 1170-1200 ℃ at the speed of 10-30 ℃/h, and keeping the temperature for 12-48 h; cooling to below 750 ℃ at a speed of less than or equal to 50 ℃/h, and then cooling in a furnace to below 200 ℃ for air cooling; wherein T satisfies: t is more than or equal to Ts-20 ℃ and less than or equal to Ts +20 ℃, and the Ts is the total-solution temperature of the reinforcement phase gamma prime phase;
the grain size of the pre-cogging treated blank is 2-7 grades; the grain size of the forging stock after cogging forging is 8 grades or thinner;
the high-alloying high-temperature alloy comprises the following chemical components in percentage by mass: 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: less than or equal to 1 percent, and the balance of Ni and inevitable impurities.
2. The method of homogenizing a high alloy material according to claim 1, wherein the number of fire cycles in the pre-cogging forging is 1 to 3.
3. The method of homogenizing a high alloy material as claimed in claim 2, wherein the amount of deformation per firing in the pre-cogging forging is 15% to 45%.
4. The method for homogenization of high alloy superalloy material of claim 1, wherein the cogging forging is performed with constrained upsetting.
5. The method of homogenizing a high alloy superalloy material as in claim 1, wherein the cogging forging is performed as a multi-directional forging.
6. The method for homogenizing a high alloy superalloy material according to claim 1, wherein in the cogging forging, the forging temperature is 950 to 1170 ℃.
7. The method for homogenizing a high alloy superalloy material according to claim 1, wherein the amount of deformation per firing in the cogging forging is 30% to 60%.
8. The method of homogenizing a high alloy material according to claim 1, wherein the diameter dimension of the high alloy ingot does not exceed 450 mm.
9. The method of homogenizing a high alloy material according to claim 1, wherein the preparing of the high alloy ingot comprises: preparing materials according to alloy components, preparing an electrode by adopting vacuum induction melting, and then smelting an ingot by adopting electroslag remelting and/or vacuum consumable remelting.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111386023.7A CN114032481B (en) | 2021-11-22 | 2021-11-22 | Method for homogenizing high-alloying high-temperature alloy material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111386023.7A CN114032481B (en) | 2021-11-22 | 2021-11-22 | Method for homogenizing high-alloying high-temperature alloy material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114032481A CN114032481A (en) | 2022-02-11 |
| CN114032481B true CN114032481B (en) | 2022-05-17 |
Family
ID=80138325
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111386023.7A Active CN114032481B (en) | 2021-11-22 | 2021-11-22 | Method for homogenizing high-alloying high-temperature alloy material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114032481B (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115245996B (en) * | 2022-03-09 | 2023-09-19 | 江西宝顺昌特种合金制造有限公司 | UNS N06030 corrosion-resistant alloy forging and preparation method thereof |
| CN114672696B (en) * | 2022-03-21 | 2023-03-14 | 钢铁研究总院有限公司 | Ni-Co-based high-temperature alloy and preparation method and application thereof |
| CN114700451B (en) * | 2022-03-28 | 2023-11-03 | 江西宝顺昌特种合金制造有限公司 | Forging production process of Waspaloy nickel-based alloy |
| CN114669701B (en) * | 2022-03-30 | 2023-10-03 | 江西宝顺昌特种合金制造有限公司 | GH4080A high-temperature alloy forging and preparation method thereof |
| CN114682718B (en) * | 2022-03-30 | 2023-10-20 | 江西宝顺昌特种合金制造有限公司 | HB-2 alloy forging and preparation method thereof |
| CN114833284B (en) * | 2022-03-30 | 2023-10-13 | 江西宝顺昌特种合金制造有限公司 | GH4145 alloy forging and preparation method thereof |
| CN114807646B (en) * | 2022-05-10 | 2023-12-05 | 山西太钢不锈钢股份有限公司 | Nickel-based alloy plate blank and preparation method thereof |
| CN115141911A (en) * | 2022-07-05 | 2022-10-04 | 中国科学院金属研究所 | Method for improving or eliminating alloy segregation and coarse precipitated phase and alloy |
| CN115354253B (en) * | 2022-09-29 | 2023-01-20 | 北京钢研高纳科技股份有限公司 | GH4780 alloy forging with high oxidation resistance and preparation method thereof |
| CN115747577B (en) * | 2022-11-21 | 2024-04-12 | 北京钢研高纳科技股份有限公司 | Deformed superalloy for turbine disk and preparation method thereof |
| CN117564200A (en) * | 2023-12-29 | 2024-02-20 | 江苏美特林科特殊合金股份有限公司 | Preparation method of short-process alloy forging |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5120373A (en) * | 1991-04-15 | 1992-06-09 | United Technologies Corporation | Superalloy forging process |
| CN106862447A (en) * | 2017-03-07 | 2017-06-20 | 钢铁研究总院 | A kind of multiway forging method of high-alloying high temperature alloy bar stock/biscuit |
| CN110449541A (en) * | 2019-07-31 | 2019-11-15 | 西部超导材料科技股份有限公司 | A kind of free forging rod billet of GH4169 high temperature alloy and preparation method thereof |
| CN110695282A (en) * | 2019-10-22 | 2020-01-17 | 成都先进金属材料产业技术研究院有限公司 | Preparation method of GH3128 alloy bar |
| CN112746231A (en) * | 2020-12-29 | 2021-05-04 | 北京钢研高纳科技股份有限公司 | Production process for gamma' phase pre-conditioning plasticization of high-performance high-temperature alloy |
| CN113235030A (en) * | 2021-05-20 | 2021-08-10 | 西安聚能高温合金材料科技有限公司 | Preparation method of large-size GH4169 high-temperature alloy bar |
-
2021
- 2021-11-22 CN CN202111386023.7A patent/CN114032481B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5120373A (en) * | 1991-04-15 | 1992-06-09 | United Technologies Corporation | Superalloy forging process |
| CN106862447A (en) * | 2017-03-07 | 2017-06-20 | 钢铁研究总院 | A kind of multiway forging method of high-alloying high temperature alloy bar stock/biscuit |
| CN110449541A (en) * | 2019-07-31 | 2019-11-15 | 西部超导材料科技股份有限公司 | A kind of free forging rod billet of GH4169 high temperature alloy and preparation method thereof |
| CN110695282A (en) * | 2019-10-22 | 2020-01-17 | 成都先进金属材料产业技术研究院有限公司 | Preparation method of GH3128 alloy bar |
| CN112746231A (en) * | 2020-12-29 | 2021-05-04 | 北京钢研高纳科技股份有限公司 | Production process for gamma' phase pre-conditioning plasticization of high-performance high-temperature alloy |
| CN113235030A (en) * | 2021-05-20 | 2021-08-10 | 西安聚能高温合金材料科技有限公司 | Preparation method of large-size GH4169 high-temperature alloy bar |
Non-Patent Citations (3)
| Title |
|---|
| 《新型铸&锻GH4198合金组织特征及偏析行为》;李福林;《稀有金属》;20200831(第8期);第807-815页 * |
| 《镍基变形高温合金开坯工艺研究进展》;陈悦;《现代冶金》;20151231(第6期);第1-5页 * |
| 《高温合金铸锭均匀化程度对开坯热变形的再结晶影响》;董建新;《金属学报》;20151031(第10期);第1207-1218页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114032481A (en) | 2022-02-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114032481B (en) | Method for homogenizing high-alloying high-temperature alloy material | |
| WO2021174727A1 (en) | Method for preparing nickel-based deformed high-temperature alloy turbine disk forging for high temperature use | |
| Qi et al. | Effect of directional solidification of electroslag remelting on the microstructure and primary carbides in an austenitic hot-work die steel | |
| EP3009525A1 (en) | Aluminium alloy forging and method for producing the same | |
| EP3327158B1 (en) | Method for producing ni-based superalloy material | |
| CN106636759B (en) | A kind of high thermal stability high-strength nickel based single-crystal high-temperature alloy that platinum family element is strengthened | |
| CN106756249A (en) | A kind of nickel-base high-temperature single crystal alloy of high intensity and tissue stabilization and preparation method thereof | |
| CN114082876B (en) | High-temperature-resistant and high-durability alloy turbine disc forging and preparation method thereof | |
| CN109022925B (en) | Method for reducing Laves phase in nickel-based superalloy steel ingot | |
| CN115156471B (en) | Preparation method of high Jiang Nieji high-temperature alloy material disc and shaft forge piece | |
| CN113877982B (en) | Hardly-deformable GH4720Li high-temperature alloy small-size bar, preparation method and blade forging | |
| CN106337145B (en) | Nickel-chromium-molybdenum alloy and method for producing same | |
| CN111440967B (en) | High-thermal-stability high-strength Re-free nickel-based single crystal superalloy and preparation process thereof | |
| CN114395717A (en) | Co-Ni-Cr-Fe-W high-density high-plasticity high-entropy alloy and preparation method thereof | |
| Guimarães et al. | Influence of yttrium addition on the microstructural evolution and mechanical properties of superalloy 718 | |
| JP2022511276A (en) | High-strength fastener material made of forged titanium alloy and its manufacturing method | |
| Cui et al. | Microstructual evolution and stability of second generation single crystal nickel-based superalloy DD5 | |
| CN113943909A (en) | Method for improving thermoplasticity of GH141 high-temperature alloy difficult to deform | |
| CN111455221B (en) | Cobalt-based high-temperature alloy for additive manufacturing, preparation method and application thereof, and additive manufactured product | |
| CN113957365A (en) | Heat treatment process for casting precipitation strengthening nickel-based high-temperature alloy | |
| CN113862520B (en) | GH4720Li high-temperature alloy for aero-engine forged blade, preparation method and application thereof, and alloy ingot | |
| Li et al. | Solidification characteristics and high temperature tensile properties of Ni-based superalloy IN713C | |
| CN107974632B (en) | Austenite hot-work die steel and preparation method thereof | |
| CN106636850B (en) | High-temperature oxidation resistance high intensity mixes rare-earth alloy material and preparation method | |
| Zhang et al. | Microstructure control and mechanical properties of new developed C&W superalloy GH4175 at 800° C |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |