CN111471897B - Preparation and forming process of high-strength nickel-based high-temperature alloy - Google Patents
Preparation and forming process of high-strength nickel-based high-temperature alloy Download PDFInfo
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Abstract
A high-strength nickel-based high-temperature alloy preparation and forming process comprises the following alloy components in percentage by mass: cr: 15-18%, Co: 15-20%, Ti: 0.5-1.5%, Al: 3.5-4.5%, W: 8.5-10%, Si: less than or equal to 0.5 percent, Mn: less than or equal to 0.5 percent, Nb: 0.5-1.5%, C: 0.03-0.08%, and the balance of Ni; the preparation process comprises three steps of alloy smelting, cogging and forging and heat treatment. And forging at high temperature for multiple times and small deformation to obtain an incomplete recrystallization texture structure. The alloy still shows obvious segregation phenomenon in the interior after heat treatment, the grain size is 70-120mm, and Ni is dispersed and distributed in the crystal3Al phase, and the volume fraction of the Al phase is not less than 35%. Meanwhile, the alloy has excellent high-temperature strength performance, the yield strength of the alloy is not lower than 700MPa at 850 ℃, and the extrapolated endurance strength at 850 ℃/100MPa is not lower than one hundred thousand hours.
Description
Technical Field
The invention belongs to the field of high-temperature alloy materials, and particularly relates to a preparation and forming process of a high-strength nickel-based high-temperature alloy.
Background
With the increasing demand of electricity in China, the problems of energy shortage and environmental pollution are increasingly highlighted, and the demand for developing efficient, energy-saving and environment-friendly power generation modes is more urgent. Thermal power generation is the most important power generation technology in China for a long time, and the improvement of steam parameters of a unit is considered to be the most effective way for solving the problems. A great deal of past practice shows that the service performance of the material of the key component is the most main reason for restricting the improvement of steam parameters of the boiler unit, and as one of the key components with the severest service working conditions in the boiler of the thermal power unit, the pass/reheater pipeline puts an extremely high requirement on the service performance of the material. The over/reheater will bear the influence of multiple factors such as high temperature creep, thermal fatigue, oxidation and high temperature flue gas corrosion during the service period. With the great improvement of main steam parameters of thermal power generating units, the development of high-temperature alloy materials capable of meeting the use performance requirements of the high-parameter unit superheater/reheater tubes has become an urgent problem to be solved in the thermal power generation industry.
The pass/reheater is used as the part with the severest service working condition in the boiler of the thermal power generating unit, and provides extremely high requirements for the lasting strength of candidate materials. In response to the demand of high-parameter boiler reheater tubes for the use of materials, a series of nickel-based wrought superalloy materials have been developed abroad, such as Inconel 740H developed by U.S. special metals, Haynes282 developed by U.S. hardson, CCA 617 developed by dernational cripper, Nimonic 263 developed by Rolls-Royce in england, FENIX700 developed by japanese hitachi, TOS1X developed by toshiba in japan, and LTESR700 developed by mitsubishi in japan. In order to ensure that the alloy has excellent endurance strength, the current candidate materials often have higher contents of Al and Ti elements. However, although the addition of Al and Ti elements is helpful for the precipitation of strengthening phases, the latter is difficult to avoid the phenomenon of coarsening and growth in the long-term service process of the alloy, thereby causing serious damage to the performance of the alloy. Some new alloys developed in recent years, such as Haynes282/usc800 and the like, have higher content of W, Mo and other solid solution strengthening elements, and contribute to reducing the thermal expansion coefficient of the alloy while improving the endurance quality of the alloy. However, the addition of Mo elements adversely affects the corrosion resistance of the alloy and significantly compromises the structural stability of the alloy. The solid solution strengthening effect of the W element is more obvious than that of the Mo element, but the addition of the W element obviously reduces the hot working performance of the alloy, and further increases the difficulty in preparing and forming the alloy.
Disclosure of Invention
The invention aims to provide a preparation and forming process of a high-strength nickel-based high-temperature alloy.
In order to achieve the above purpose, the invention adopts the technical scheme that:
a preparation and forming process of a high-strength nickel-based superalloy comprises the following steps:
1) alloy smelting: smelting the alloy raw material to obtain an ingot; wherein, the alloy comprises the following raw materials in percentage by mass: cr: 15-18%, Co: 15-20%, Ti: 0.5-1.5%, Al: 3.5-4.5%, W: 8.5-10%, Si: less than or equal to 0.5 percent, Mn: less than or equal to 0.5 percent, Nb: 0.5-1.5%, C: 0.03-0.08%, and the balance of Ni;
2) cogging and forging: homogenizing the cast ingot, and then performing cogging forging at 1180-1200 ℃, wherein the deformation of each pass is 10-15%, and the total deformation is not lower than 70%;
3) and (6) heat treatment.
The invention further improves the method that in the step 1), smelting is carried out under the protection of argon.
The further improvement of the invention is that in the step 1), a vacuum induction smelting furnace adopting a magnesia alkaline furnace lining is smelted.
The further improvement of the invention is that in the step 2), the temperature of the homogenization treatment is 1160-1200 ℃, and the time is 8-24 h.
The further improvement of the invention is that in the step 2), the temperature is increased from room temperature to 1160-1200 ℃ at the speed of 10-20 ℃/min.
The further improvement of the invention is that the ingot obtained in the step 1) is kept at the temperature of 950 ℃ and 1020 ℃ for 0.5-1.5 hours before the step 2) is carried out.
The further improvement of the invention is that in the step 2), the furnace returns and the heat preservation are carried out after each time of cogging forging is finished, and the heat preservation time T and the time T outside the furnace meet the condition that T is less than or equal to 10T.
The further improvement of the invention is that in the step 3), the specific process of the heat treatment is as follows: and (3) preserving the heat of the alloy after cogging forging for 0.5-2.0 hours at 1150-1180 ℃, then air-cooling, preserving the heat for 0.5-1.5 hours at 980-1050 ℃, then air-cooling, preserving the heat for 7-9 hours at 750-770 ℃, then preserving the heat for 1.5-2.5 hours at 840-870 ℃, and finally air-cooling to room temperature.
Compared with the prior art, the invention has the following beneficial effects:
the invention develops a preparation, processing and forming process of the alloy with high W content on the basis of high strengthening phase volume fraction. Finally, the alloy structure with incomplete recrystallization is obtained, and meanwhile, the excellent strength, corrosion/oxidation resistance and structure stability of the alloy structure are ensured. The alloy is forged at high temperature by adopting a preparation process with multiple passes and small deformation, and the external processing temperature and time are strictly controlled, so that the deformation temperature of the alloy is ensured to be within a reasonable range. Finally obtaining the nickel-based high-tungsten polycrystalline superalloy with isotropy through high-temperature forging
The alloy prepared by the forming process of the invention is not completely recrystallized after heat treatment, obvious segregation can still be seen in the alloy, the grain size is 70-120mm, and Ni is dispersed and distributed in the crystal3Al phase, and the volume fraction of the Al phase is not less than 35%. Meanwhile, the alloy has excellent high-temperature strength performance, the yield strength of the alloy is not lower than 700MPa at 850 ℃, and the extrapolated endurance strength at 850 ℃/100MPa is not lower than one hundred thousand hours.
Further, the ingot obtained in the step 1) is kept at 950 ℃ and 1020 ℃ for 0.5-1.5 hours to ensure that the low-melting phase is completely dissolved.
Drawings
FIG. 1 is a photograph of a hot-forged plate material of example 1.
FIG. 2 is a photograph of the tissue of example 1.
FIG. 3 shows Ni in example 13And (5) an Al precipitated phase morphology graph.
FIG. 4 is a photograph of a hot-forged plate of comparative example 1.
Fig. 5 is a photograph of the structure of comparative example 1.
Detailed Description
The present invention will be described in further detail with reference to examples.
The invention provides a preparation and forming process of a high-strength nickel-based high-temperature alloy, which comprises three steps of alloy smelting, cogging forging and heat treatment, and specifically comprises the following steps:
1) alloy smelting: smelting the prepared alloy raw material by using a vacuum induction smelting furnace, and introducing high-purity argon gas for smelting when the vacuum degree reaches the range of 0.3-0.5 Pa; wherein the alloy raw material comprises the following components in percentage by mass: cr: 15-18%, Co: 15-20%, Ti: 0.5-1.5%, Al: 3.5-4.5%, W: 8.5-10%, Si: less than or equal to 0.5 percent, Mn: less than or equal to 0.5 percent, Nb: 0.5-1.5%, C: 0.03-0.08%, and the balance of Ni;
the magnesium oxide alkaline furnace lining is adopted for alloy smelting, a pure nickel furnace washing is adopted before the smelting, shot blasting is carried out before the alloy raw materials are added, and the P, S content is not higher than 0.03% at the later stage of alloy smelting;
2) cogging and forging: heating the cast ingot to 1160-1200 ℃ at the speed of 10-20 ℃/min for homogenization treatment, and then performing cogging forging at 1180-1200 ℃, wherein the deformation of each pass is 10-15%, and the total deformation is not lower than 70%; the alloy should be kept at 950 ℃ and 1020 ℃ for 0.5-1.5 hours before being heated to the homogenization treatment temperature to ensure that the low melting point phase is completely dissolved. Meanwhile, the forging of each pass is finished, the forging is returned to the furnace and the temperature is preserved, and the heat preservation time T and the time T outside the furnace meet the condition that T is not less than 10T;
3) and (3) heat treatment: keeping the temperature of the rolled alloy at 1150-1180 ℃ for 0.5-2.0 hours, then air-cooling, keeping the temperature at 980-1050 ℃ for 0.5-1.5 hours, then air-cooling, keeping the temperature at 750-770 ℃ for 7-9 hours, air-cooling, keeping the temperature at 840-870 ℃ for 1.5-2.5 hours, and finally air-cooling to room temperature;
the alloy is not completely recrystallized after heat treatment, obvious segregation can still be seen in the alloy, the grain size is 70-120mm, and Ni is dispersed and distributed in the crystal3Al phase, and the volume fraction of the Al phase is not less than 35%. Meanwhile, the alloy has excellent high-temperature strength performance, the yield strength of the alloy is not lower than 700MPa at 850 ℃, and the extrapolated endurance strength at 850 ℃/100MPa is not lower than one hundred thousand hours.
Example 1
The heat-resistant steel material of the embodiment includes, by mass: cr: 17%, Co: 20%, Ti: 1.5%, Al: 4.5%, W: 8.5%, Si: 0.2%, Mn: 0.3%, Nb: 1.5%, C: 0.06 percent, and the balance of Ni;
the forming preparation process of the embodiment comprises three steps of alloy smelting, cogging and forging and heat treatment:
1) alloy smelting: and smelting the prepared alloy raw materials by adopting a vacuum induction smelting furnace, and introducing high-purity argon gas for smelting when the vacuum degree reaches the range of 0.35 Pa. Wherein, the alloy smelting adopts a magnesia alkaline furnace lining, a pure nickel furnace washing is adopted before the smelting, and shot blasting is carried out before the alloy raw materials are added, so that the P, S content in the later stage of alloy smelting is not higher than 0.03%;
2) cogging and forging: heating the cast ingot to 1200 ℃ at the speed of 10 ℃/min for homogenization treatment, and then performing cogging forging at the temperature of 1180-1200 ℃, wherein the deformation of each pass is 15 percent, and the total deformation is 75 percent. Wherein the alloy is kept at 950 ℃ for 0.5 hour before being heated to the homogenization treatment temperature, and is returned to the furnace for heat preservation after each forging, and the heat preservation time T and the time T outside the furnace meet the condition that T is not more than 10T;
3) and (3) heat treatment: keeping the rolled alloy at 1180 ℃ for 2.0 hours, then air-cooling, keeping the temperature at 1020 ℃ for 0.5 hour, then air-cooling, keeping the temperature at 760 ℃ for 8 hours, keeping the temperature at 860 ℃ for 2 hours, and finally air-cooling to room temperature;
FIG. 1 is a photograph of a hot forged plate of example 1, which was formed by forging an alloy with a small deformation in a plurality of passes.
FIG. 2 is a microstructure morphology of the alloy after forging and heat treatment, which is seen to consist of coarse equiaxed grains with an average size of about 100 microns, but still with significant macrosegregation visible within the interior, indicating incomplete recrystallization of the alloy.
FIG. 3 shows Ni in example 13The appearance of Al precipitated phase shows that a large amount of strengthening phase is uniformly dispersed and precipitated in the crystal grains after the heat treatment of the alloy, and the average size of the strengthening phase is within the range of 30-50 nm. The mechanical property test result after the heat treatment of the alloy shows that the alloy has 714MPa of yield strength at 850 ℃.
Example 2
The heat-resistant steel material of the embodiment includes, by mass: cr: 16%, Co: 20%, Ti: 1.2%, Al: 4.2%, W: 10%, Si: 0.3%, Mn: 0.3%, Nb: 1.0%, C: 0.05 percent, and the balance being Ni;
the preparation forming process of the embodiment comprises three steps of alloy smelting, cogging and forging and heat treatment:
1) alloy smelting: and smelting the prepared alloy raw materials by adopting a vacuum induction smelting furnace, and introducing high-purity argon gas for smelting when the vacuum degree reaches the range of 0.35 Pa. Wherein, the alloy smelting adopts a magnesia alkaline furnace lining, a pure nickel furnace washing is adopted before the smelting, and shot blasting is carried out before the alloy raw materials are added, so that the P, S content in the later stage of alloy smelting is not higher than 0.03%;
2) cogging and forging: heating the cast ingot to 1200 ℃ at the speed of 10 ℃/min for homogenization treatment, and then performing cogging forging at the temperature of 1180-1200 ℃, wherein the deformation of each pass is 10% and the total deformation is 70%. Wherein the alloy is kept at 950 ℃ for 0.5 hour before being heated to the homogenization treatment temperature, and is returned to the furnace for heat preservation after each forging, and the heat preservation time T and the time T outside the furnace meet the condition that T is not more than 10T;
3) and (3) heat treatment: keeping the rolled alloy at 1180 ℃ for 2.0 hours, then air-cooling, keeping the temperature at 1020 ℃ for 0.5 hour, then air-cooling, keeping the temperature at 760 ℃ for 8 hours, keeping the temperature at 860 ℃ for 2 hours, and finally air-cooling to room temperature;
example 3
1) Alloy smelting: vacuumizing, and smelting the alloy raw material by using a vacuum induction smelting furnace with a magnesium oxide alkaline furnace lining under the protection of argon to obtain an ingot; wherein, the alloy comprises the following raw materials in percentage by mass: cr: 16%, Co: 20%, Ti: 0.5%, Al: 3.5%, W: 10%, Si: 0.5%, Mn: 0.5%, Nb: 0.5%, C: 0.03 percent, and the balance being Ni;
2) cogging and forging: keeping the temperature of the cast ingot at 950 ℃ for 1.5 hours, then heating the cast ingot from room temperature to 1180 ℃ at the speed of 10 ℃/min for homogenization treatment for 15 hours, then performing cogging forging at 1180 ℃, wherein the deformation of each pass is 15 percent, the cast ingot is returned to the furnace for heat preservation after each pass of cogging forging is completed, the heat preservation time T and the time T outside the furnace meet the condition that the T is less than or equal to 10T, and the total deformation is not less than 70 percent;
3) and (3) heat treatment: the alloy after cogging and forging is kept at 1150 ℃ for 2.0 hours and then cooled in air, then kept at 980 ℃ for 1.5 hours and then cooled in air, then kept at 750 ℃ for 9 hours and then cooled in air, and then kept at 840 ℃ for 2.5 hours and finally cooled in air to room temperature.
Example 4
1) Alloy smelting: vacuumizing, and smelting the alloy raw material by using a vacuum induction smelting furnace with a magnesium oxide alkaline furnace lining under the protection of argon to obtain an ingot; wherein, the alloy comprises the following raw materials in percentage by mass: cr: 18%, Co: 15%, Ti: 1%, Al: 4%, W: 9%, Si: 0.3%, Mn: 0.5%, Nb: 1%, C: 0.08 percent, and the balance being Ni;
2) cogging and forging: keeping the temperature of the cast ingot at 1000 ℃ for 1 hour, then heating the cast ingot from room temperature to 1160 ℃ at the speed of 20 ℃/min for homogenization treatment for 24 hours, then performing cogging forging at 1200 ℃, wherein the deformation of each pass is 10 percent, returning to the furnace and keeping the temperature after each pass of cogging forging is completed, the heat preservation time T and the time T outside the furnace meet the condition that the T is not more than 10T, and the total deformation is not less than 70 percent;
3) and (3) heat treatment: keeping the temperature of the alloy after cogging forging at 1160 ℃ for 1.0 hour, then cooling in air, keeping the temperature at 1050 ℃ for 0.5 hour, then cooling in air, keeping the temperature at 770 ℃ for 8 hours, then cooling in air, keeping the temperature at 870 ℃ for 1.5 hours, and finally cooling in air to room temperature.
Example 5
1) Alloy smelting: vacuumizing, and smelting the alloy raw material by using a vacuum induction smelting furnace with a magnesium oxide alkaline furnace lining under the protection of argon to obtain an ingot; wherein, the alloy comprises the following raw materials in percentage by mass: cr: 15%, Co: 17%, Ti: 1.5%, Al: 4.5%, W: 8.5%, Mn: 0.2%, Nb: 1.5%, C: 0.05 percent, and the balance being Ni;
2) cogging and forging: keeping the temperature of the cast ingot at 1020 ℃ for 0.5 hour, then heating the cast ingot from room temperature to 1200 ℃ at the speed of 15 ℃/min for homogenization treatment for 8 hours, then performing cogging forging at 1200 ℃, wherein the deformation of each pass is 10 percent, the cast ingot is returned to the furnace for heat preservation after each pass of cogging forging is completed, the heat preservation time T and the time T outside the furnace meet the condition that the T is not more than 10T, and the total deformation is not less than 70 percent;
3) and (3) heat treatment: keeping the temperature of the alloy after cogging forging at 1180 ℃ for 0.5 hour, then air-cooling the alloy after keeping the temperature at 1020 ℃ for 1 hour, then air-cooling the alloy after keeping the temperature at 760 ℃ for 7 hours, then keeping the temperature at 850 ℃ for 2 hours, and finally air-cooling the alloy to room temperature.
Comparative example 1
The heat-resistant steel material of the embodiment includes, by mass: cr: 17%, Co: 20%, Ti: 1.5%, Al: 4.5%, W: 8.5%, Si: 0.2%, Mn: 0.3%, Nb: 1.5%, C: 0.06 percent, and the balance of Ni;
the preparation forming process of the embodiment comprises three steps of alloy smelting, cogging and forging and heat treatment:
1) alloy smelting: and smelting the prepared alloy raw materials by adopting a vacuum induction smelting furnace, and introducing high-purity argon gas for smelting when the vacuum degree reaches the range of 0.35 Pa. Wherein, the alloy smelting adopts a magnesia alkaline furnace lining, a pure nickel furnace washing is adopted before the smelting, and shot blasting is carried out before the alloy raw materials are added, so that the P, S content in the later stage of alloy smelting is not higher than 0.03%;
2) cogging and forging: heating the cast ingot to 1200 ℃ at the speed of 10 ℃/min for homogenization treatment, and then performing cogging forging at the temperature of 1180-1200 ℃, wherein the deformation of each pass is 20 percent, and the total deformation is 55 percent. Wherein the alloy is heated to the homogenization treatment temperature and then is kept at 950 ℃ for 0.5 hour, and simultaneously, the alloy is returned to the furnace for heat preservation after each forging, and the heat preservation time T and the time T outside the furnace meet the condition that T is not more than 10T;
3) and (3) heat treatment: keeping the temperature of the rolled alloy at 1120 ℃ for 4.0 hours, then air-cooling, keeping the temperature at 1020 ℃ for 0.5 hour, air-cooling, keeping the temperature at 760 ℃ for 8 hours, keeping the temperature at 860 ℃ for 2 hours, and finally air-cooling to room temperature;
FIG. 4 is a photograph of a hot forged plate of comparative example 1, in which the temperature drop amplitude is too large due to too long forging time after the deformation of each pass of the alloy is increased, so that the workability is reduced, and meanwhile, the deformation difficulty is further increased due to the work hardening of the alloy due to the large deformation, so that a large number of cracks are initiated in the forging process.
FIG. 5 is a photograph of the structure of the alloy of comparative example 1, in which the lower solution treatment temperature resulted in a slower growth rate of the recrystallization manager, and the average grain size did not exceed 50 μm. The mechanical property test result after the heat treatment of the alloy shows that the yield strength of the alloy is only 631MPa at 850 ℃.
Table 1 shows the results of the endurance strength performance test of example 1 and comparative example 1. It can be seen that the endurance strength of example 1 is improved by more than 80% compared with that of comparative example 1, and the 850 ℃/100MPa extrapolated endurance life of the composite material reaches one hundred thousand hours.
Table 1 results of the endurance strength performance test of example 1 and comparative example 1.
According to the invention, the alloy structure is improved and controlled by the multi-pass small-deformation cogging forging temperature and the deformation in a reasonable temperature range, and finally the nickel-based polycrystalline high-temperature alloy plate with high tungsten content is obtained. The alloy is an incomplete recrystallization structure after final heat treatment, obvious segregation can still be seen in the alloy, the grain size is 70-120mm, and Ni is dispersed and distributed in the alloy3Al phase, and the volume fraction of the Al phase is not less than 35%. Meanwhile, the alloy has excellent high-temperature strength performance, the yield strength of the alloy is not lower than 700MPa at 850 ℃, and the extrapolated endurance strength at 850 ℃/100MPa is not lower than one hundred thousand hours.
Claims (2)
1. A preparation and forming process of a high-strength nickel-based superalloy is characterized by comprising the following steps:
1) alloy smelting: smelting the alloy raw material under the protection of argon to obtain an ingot; wherein, the alloy comprises the following raw materials in percentage by mass: cr: 15-18%, Co: 15-20%, Ti: 0.5-1.5%, Al: 3.5-4.5%, W: 9-10%, Si: less than or equal to 0.5 percent, Mn: less than or equal to 0.5 percent, Nb: 0.5-1.5%, C: 0.03-0.08%, and the balance of Ni;
2) cogging and forging: heating the cast ingot from room temperature to 1160-1200 ℃ at the speed of 10-20 ℃/min for homogenization treatment for 8-24h, and then performing cogging forging at 1180-1200 ℃, wherein the deformation of each pass is 10-15%, and the total deformation is not lower than 70%; keeping the temperature at 1020 ℃ of 950-;
3) and (3) heat treatment: the specific process is to make the alloy after cogging and forging in 1150-1180oC, air cooling after heat preservation for 0.5-2.0 hours, then air cooling after heat preservation for 0.5-1.5 hours at 980-1050 ℃, and then air cooling at 750-770oC, preserving heat for 7-9 hours, air-cooling, and then 840-870oAnd C, preserving the heat for 1.5-2.5 hours, and finally cooling to room temperature in air.
2. The process for preparing and forming the high-strength nickel-based superalloy according to claim 1, wherein in the step 1), a vacuum induction melting furnace with a magnesium oxide alkaline lining is used for melting.
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| JP6012454B2 (en) * | 2012-12-21 | 2016-10-25 | 三菱日立パワーシステムズ株式会社 | Forged member and steam turbine rotor, steam turbine rotor blade, boiler piping, boiler tube and steam turbine bolt using the same |
| CN110106398B (en) * | 2019-06-14 | 2020-08-18 | 中国华能集团有限公司 | Low-chromium corrosion-resistant high-strength polycrystalline high-temperature alloy and preparation method thereof |
| CN110157993B (en) * | 2019-06-14 | 2020-04-14 | 中国华能集团有限公司 | High-strength corrosion-resistant iron-nickel-based high-temperature alloy and preparation method thereof |
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