CN107805770B - Overaging heat treatment process suitable for casting high-temperature alloy - Google Patents
Overaging heat treatment process suitable for casting high-temperature alloy Download PDFInfo
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Abstract
An overaging heat treatment process suitable for casting a superalloy, comprising the steps of: carrying out solid solution treatment on the cast high-temperature alloy, then carrying out high-temperature aging treatment, and finally carrying out low-temperature aging treatment; wherein the high-temperature aging treatment comprises the specific processes of completing solution treatment, cooling to 50-150 ℃ below the gamma' phase solution temperature, preserving heat for no more than 3 hours, and then cooling to room temperature. Compared with the cast high-temperature alloy treated by the process in an as-cast state, the yield strength of the cast high-temperature alloy at 750 ℃ is improved by 3-10%, and the elongation is improved by 90-120%; compared with the alloy in a heat treatment state without high-temperature aging, the yield strength of the alloy is reduced by not more than 10% at 750 ℃, and the elongation is improved by 60-100%.
Description
Technical Field
The invention belongs to the technical field of metal heat treatment, and particularly relates to an overaging heat treatment process suitable for casting high-temperature alloy.
Background
The fine gamma' phase is dispersed and precipitated uniformly in the crystal grains, which is an important guarantee for ensuring the excellent high-temperature strength of the alloy. At present, high-temperature materials taking a gamma' phase as a main strengthening phase are widely applied to a plurality of fields of energy, electric power, aerospace and the like, and obtain good use effects. The increase of the volume fraction of the gamma' phase is an effective way for further improving the high-temperature strength of the alloy. However, this also causes great difficulty in high-temperature deformation of the alloy, resulting in a drastic increase in the manufacturing cost of processing high-temperature parts having more complicated shapes. This is because the heat distortion temperature of high temperature alloys is often selected to be above the gamma prime solution temperature for good workability. While the solution temperature of the γ' phase tends to increase with an increase in its volume fraction. Therefore, the volume fraction of the gamma' phase in the alloy is increased, and simultaneously, the great difficulty is brought to the processing deformation of the alloy. In the nickel-based or iron-nickel-based high-temperature alloy which is widely applied at present, the volume fraction of a gamma 'strengthening phase generally does not exceed 20%, and with the increase of the volume fraction of the gamma' phase, the hot processing window of the alloy is obviously reduced, and the processing cost of the alloy is sharply increased.
The high-temperature alloy casting direct forming can meet the size requirement of workpieces with complex shapes. In addition, since the cast alloy can be directly formed by adopting a casting process and the later steps of cold and hot working and the like are omitted, the cast high-temperature alloy can often have a larger volume fraction gamma' so as to obtain higher strength performance of the material. However, parts produced by casting processes tend to form columnar dendrites in the solidification direction due to differences in cooling rates, and the like. Such grains having coarse dimensions are difficult to achieve a coordinated deformation effect, and therefore cast superalloys often exhibit poor plasticity compared to deformed superalloys. Particularly, when the volume fraction of the gamma' phase in the alloy is larger, the inside of the alloy crystal grain obtains higher strength, but the crystal grain is difficult to deform, so that the grain boundary sliding is difficult to generate stress concentration, and the initiation and the propagation of cracks are further promoted.
Disclosure of Invention
To overcome the problems of the prior art, the invention aims to provide an overaging heat treatment process suitable for casting high-temperature alloys.
In order to achieve the above purpose, the invention adopts the technical scheme that:
an overaging heat treatment process suitable for casting a superalloy, comprising the steps of: carrying out solid solution treatment on the cast high-temperature alloy, then carrying out high-temperature aging treatment, and finally carrying out low-temperature aging treatment; the specific process of the high-temperature aging treatment comprises the following steps: cooling to 50-150 ℃ below the gamma' phase solid solution temperature after the completion of the solid solution treatment, preserving the heat for no more than 3 hours, and then cooling to room temperature by air.
In a further development of the invention, the cast superalloy is a nickel-iron-based or nickel-based superalloy.
In a further improvement of the invention, the cast superalloy has a gamma prime volume fraction of not less than 15% at thermodynamic equilibrium.
The further improvement of the invention is that the cooling is carried out at a speed of 5-15 ℃/min to a temperature which is 50-150 ℃ below the solid solution temperature of the gamma' phase.
The invention further improves the method that the specific process of the solution treatment is as follows: the cast high-temperature alloy is kept for 20min to 60min at the temperature of 30 ℃ to 50 ℃ above the gamma 'phase solid solution temperature, heated to 150 ℃ to 350 ℃ above the gamma' phase solid solution temperature and kept for 0.5 to 2 hours.
The invention is further improved in that the temperature is increased to be higher than the gamma' phase solid solution temperature by 150 ℃ and 350 ℃ at the speed of 5-10 ℃/min.
The invention has the further improvement that the specific process of the low-temperature aging treatment is as follows: after the high-temperature aging treatment is finished, heating to the temperature of 300-400 ℃ below the gamma 'phase solid solution temperature, preserving the heat for no more than 20 hours, then heating to the temperature of 200-300 ℃ below the gamma' phase solid solution temperature, preserving the heat for 5-10 hours, and finally air cooling to the room temperature.
The invention is further improved in that the temperature is raised to be within the range of 200-300 ℃ below the gamma' phase solid solution temperature at the speed of 10-15 ℃/min.
Compared with the prior art, the invention has the following beneficial effects: the invention utilizes the principle of improving the plasticity of the alloy by overaging, and adds high-temperature aging treatment on the basis of the traditional heat treatment process of high-temperature solid solution and low-temperature aging to promote the uniform dispersion precipitation of granular primary gamma 'phases with larger size in the crystal grains, the average size of the precipitated phases is not less than 100nm, and a phase precipitated phase lean zone is ensured to be generated around the gamma' phase with large size. The appearance of the precipitated phase barren zone can promote the non-uniform deformation in the columnar crystal grains of the alloy, and further improve the capability of the coordinated deformation of the crystal grains and the crystal boundary, thereby improving the high-temperature plasticity of the alloy. Since the occurrence of the precipitated phase lean zone also causes the reduction of the alloy strength, the size, volume fraction and the width of the surrounding precipitated phase lean zone of the large-size gamma' phase are controlled by reasonably adjusting the temperature and time of the high-temperature aging treatment. Finally, the alloy is ensured to obtain a larger plasticity improving effect on the premise of controlling the alloy strength reduction amplitude, so that the alloy achieves the optimal combination of strength and plasticity. Compared with the as-cast alloy, the alloy prepared by the process has the advantages that the yield strength is improved by 3-10% at 750 ℃, and the elongation is improved by 90-120%; compared with the alloy in a heat treatment state without high-temperature aging, the yield strength of the alloy is reduced by not more than 10% at 750 ℃, and the elongation is improved by 60-100%. The invention is particularly suitable for the service working conditions which are used at the temperature of more than 700 ℃ and have relatively high requirements on the plasticity of the alloy, such as a reheater of an advanced ultra-supercritical boiler unit, a hydrogen production converter in an ethylene cracking furnace tube and the like.
Furthermore, the primary gamma' phase of the cast high-temperature alloy is completely dissolved after solution treatment, and the alloy consists of coarse austenite columnar dendrites and discontinuous carbides distributed between grain boundaries and dendrites.
Further, after low-temperature aging treatment, a granular primary gamma 'phase with a larger size and a granular secondary gamma' phase with a fine size are uniformly dispersed and precipitated in the alloy crystal grains, wherein the average size of the primary gamma 'phase is not less than 100nm, and the average size of the secondary gamma' phase is not more than 30 nm. A secondary gamma 'particle precipitation-lean zone (PFZ) is present at the primary gamma' particle edge, and the PFZ zone width does not exceed 300 nm.
Detailed Description
The invention is described in further detail below:
the cast high-temperature alloy is Fe-Ni-based or Ni-based, and the volume fraction of the gamma' phase of the cast high-temperature alloy in a thermodynamic equilibrium state is not less than 15%. The cast high-temperature alloy is prepared by adopting the components in the patent with the application number of 201310397115.4 through a centrifugal casting process.
Example 1
1) Solution treatment: the alloy comprises the following components in percentage by weight: 201310397115.4, the name is: a low-expansion antioxidizing Ni-Fe-Cr-base high-temp alloy, gamma' (Ni) as the component of high-temp alloy, is prepared through centrifugal casting3Al) phase was 984 ℃. Heating the alloy to 1000 ℃ along with the furnace, preserving heat for 30 minutes, and then heating to 1200 ℃ at the speed of 10 ℃/min for solid solution for 2 hours;
2) high-temperature aging treatment: after the solution treatment is finished, cooling to 900 ℃ at the speed of 15 ℃/min, preserving the heat for 1 hour, and then cooling to room temperature;
3) and (3) low-temperature aging treatment: and (3) feeding the alloy subjected to the high-temperature aging treatment into a furnace, heating to 650 ℃ along with the furnace, preserving heat for 16 hours, then heating to 750 ℃ at the speed of 15 ℃/min, preserving heat for 8 hours, and then air-cooling to room temperature.
Scanning electron microscope testing of the coarse austenite columnar dendrites in the cast superalloy of example 1 revealed that the cast superalloy had coarse austenite columnar dendrites.
Example 2
1) Solution treatment: the alloy comprises the following components in percentage by weight: 201310397115.4, the name is: a low-expansion antioxidizing Ni-Fe-Cr-base high-temp alloy is prepared through centrifugal casting at 984 deg.C. Heating the alloy to 1000 ℃ along with the furnace, preserving heat for 30 minutes, and then heating to 1200 ℃ at the speed of 10 ℃/min for solid solution for 2 hours;
2) high-temperature aging treatment: after the solution treatment is finished, cooling to 900 ℃ at the speed of 15 ℃/min, preserving the heat for 2 hours, and then cooling to room temperature;
3) and (3) low-temperature aging treatment: and (3) feeding the alloy subjected to the high-temperature aging treatment into a furnace, heating to 650 ℃ along with the furnace, preserving heat for 16 hours, then heating to 750 ℃ at the speed of 15 ℃/min, preserving heat for 8 hours, and then air-cooling to room temperature.
The transmission electron microscope test of the large-size gamma 'phase formed in the high-temperature aging process and the precipitated phase lean areas around the large-size gamma' phase in the example 2 shows that the large-size gamma 'phase and the precipitated phase lean areas around the large-size gamma' phase are formed in the high-temperature aging process.
Example 3
1) Solution treatment: the alloy comprises the following components in percentage by weight: 201310397115.4, the name is: a low-expansion antioxidizing Ni-Fe-Cr-base high-temp alloy is prepared through centrifugal casting at 984 deg.C. Heating the alloy to 1000 ℃ along with the furnace, preserving heat for 30 minutes, and then heating to 1200 ℃ at the speed of 10 ℃/min for solid solution for 2 hours;
2) high-temperature aging treatment: after the solution treatment is finished, cooling to 850 ℃ at the speed of 15 ℃/min, preserving the heat for 10min, and then cooling to room temperature;
3) and (3) low-temperature aging treatment: and (3) feeding the alloy subjected to the high-temperature aging treatment into a furnace, heating to 650 ℃ along with the furnace, preserving heat for 16 hours, then heating to 750 ℃ at the speed of 15 ℃/min, preserving heat for 8 hours, and then air-cooling to room temperature.
Example 4
1) Solution treatment: the alloy comprises the following components in percentage by weight: 201310397115.4, the name is: a low-expansion antioxidizing Ni-Fe-Cr-base high-temp alloy is prepared through centrifugal casting at 984 deg.C. Heating the alloy to 1000 ℃ along with the furnace, preserving heat for 30 minutes, and then heating to 1200 ℃ at the speed of 10 ℃/min for solid solution for 2 hours;
2) high-temperature aging treatment: after the solution treatment is finished, cooling to 850 ℃ at the speed of 15 ℃/min, preserving the heat for 0.5 hour, and then cooling to room temperature;
3) and (3) low-temperature aging treatment: and (3) feeding the alloy subjected to the high-temperature aging treatment into a furnace, heating to 650 ℃ along with the furnace, preserving heat for 16 hours, then heating to 750 ℃ at the speed of 15 ℃/min, preserving heat for 8 hours, and then air-cooling to room temperature.
Example 5
1) Solution treatment: the alloy comprises the following components in percentage by weight: 201310397115.4, the name is: a low-expansion antioxidizing Ni-Fe-Cr-base high-temp alloy is prepared through centrifugal casting at 984 deg.C. Heating the alloy to 1014 ℃ along with the furnace, preserving the heat for 20 minutes, and then heating to 1134 ℃ at the speed of 5 ℃/min for solid solution for 2 hours;
2) high-temperature aging treatment: after the solution treatment is finished, cooling to 850 ℃ at the speed of 5 ℃/min, preserving the heat for 20min, and then cooling to room temperature;
3) and (3) low-temperature aging treatment: and (3) feeding the alloy subjected to the high-temperature aging treatment into a furnace, heating to 684 ℃ along with the furnace, preserving heat for 1 hour, then heating to 784 ℃ at the speed of 5 ℃/min, preserving heat for 5 hours, and then cooling to room temperature in air.
Example 6
1) Solution treatment: the alloy comprises the following components in percentage by weight: 201310397115.4, the name is: a low-expansion antioxidizing Ni-Fe-Cr-base high-temp alloy is prepared through centrifugal casting at 984 deg.C. Heating the alloy to 1034 ℃ along with the furnace, preserving the heat for 60 minutes, and then heating to 1334 ℃ at the speed of 15 ℃/min for solid solution for 0.5 hour;
2) high-temperature aging treatment: after the solution treatment is finished, cooling to 850 ℃ at the speed of 10 ℃/min, preserving the heat for 40min, and then cooling to room temperature;
3) and (3) low-temperature aging treatment: and (3) feeding the alloy subjected to the high-temperature aging treatment into a furnace, heating to 584 ℃ along with the furnace, preserving the heat for 20 hours, then heating to 684 ℃ at the speed of 10 ℃/min, preserving the heat for 10 hours, and then cooling to room temperature in air.
Comparative example 1
The alloy comprises the following components in percentage by weight: 201310397115.4, the name is: the components of the low-expansion antioxidant NiFeCr-based high-temperature alloy and the preparation method thereof are used for preparing a formed alloy by adopting a centrifugal casting process.
Comparative example 2
The alloy comprises the following components in percentage by weight: 201310397115.4, the name is: a low-expansion antioxidizing Ni-Fe-Cr-base high-temp alloy is prepared through centrifugal casting to obtain a shaped alloy tube with gamma' phase dissolved at 984 deg.C. Heating the alloy to 1000 ℃ along with the furnace, preserving heat for 30 minutes, and then heating to 1200 ℃ at the speed of 10 ℃/min for solid solution for 2 hours; after the solution treatment is finished, cooling to 950 ℃ at the speed of 15 ℃/min, preserving the heat for 1 hour, and then air-cooling to room temperature; and (3) feeding the alloy subjected to the high-temperature aging treatment into a furnace, preserving heat for 16 hours at 650 ℃, then raising the temperature to 750 ℃ at the speed of 15 ℃/min, preserving heat for 8 hours, and then cooling to room temperature in air.
In the high temperature aging treatment of comparative example 2, the temperature does not satisfy the condition of cooling to the range of 50 to 150 c below the solid solution temperature of the γ ' phase and maintaining the temperature, so that after the process treatment of this comparative example, it still has only a fine γ ' phase of one particle size, and the γ ' phases of two sizes as in example 2 cannot be obtained.
Comparative example 3
The alloy comprises the following components in percentage by weight: 201310397115.4, the name is: a low-expansion antioxidizing Ni-Fe-Cr-base high-temp alloy is prepared through centrifugal casting to obtain a shaped alloy tube with gamma' phase dissolved at 984 deg.C. Heating the alloy pipe to 1000 ℃ along with a furnace, preserving heat for 30 minutes, and then heating to 1200 ℃ at the speed of 10 ℃/min for solid solution for 2 hours; after the solution treatment is finished, the alloy is sent into a furnace to be kept at 650 ℃ for 16 hours, then the temperature is raised to 750 ℃ at the speed of 15 ℃/min and kept for 8 hours, and then the alloy is cooled to room temperature in air.
Comparing example 1, example 2 and comparative example 3, it can be seen that the alloy as-cast structure is composed of coarse austenite grains, and γ 'phases having large and small sizes are precipitated inside the alloy grains after high-temperature aging, respectively, and a precipitated phase lean region occurs around the large-size γ' phase. The maximum width of the precipitate phase barren zone is not more than 300 nm. The alloy which is not subjected to high temperature ageing only has small-size gamma 'phase inside the crystal grains, and the average size of the gamma' phase is not more than 50 nm.
The alloys of examples 1-4 and comparative examples 1-3 were tested for plasticity and strength according to the present invention and are shown in Table 1.
TABLE 1
As can be seen from Table 1, the high temperature performance of the alloy after heat treatment is greatly improved, and compared with the alloy without heat treatment, the plasticity of the alloy after high temperature aging treatment is obviously improved, and the strength is slightly reduced.
The nickel-iron-based high-temperature alloy is taken as an example for explanation in the embodiments 1 to 6 of the invention, and the nickel-based high-temperature alloy can also achieve the purpose of the invention through the process of the invention.
Claims (2)
1. An overaging heat treatment process suitable for casting high-temperature alloy is characterized in that the cast high-temperature alloy is subjected to solid solution treatment, then high-temperature aging treatment and finally low-temperature aging treatment; the specific process of the high-temperature aging treatment comprises the following steps: after the solution treatment is finished, cooling to the temperature which is 50-150 ℃ below the gamma' phase solution temperature at the speed of 5-15 ℃/min, preserving the heat for no more than 3 hours, and then air-cooling to the room temperature; wherein the solid solution treatment comprises the following specific processes: keeping the temperature of the cast high-temperature alloy within the range of 30-50 ℃ above the gamma 'phase solid solution temperature for 20-60 min, then raising the temperature to be 150-350 ℃ above the gamma' phase solid solution temperature at the speed of 5-10 ℃/min and keeping the temperature for 0.5-2 h; the specific process of the low-temperature aging treatment comprises the following steps: after the high-temperature aging treatment is finished, heating to the temperature of 300-400 ℃ below the gamma 'phase solid solution temperature, preserving the heat for no more than 20 hours, then heating to the temperature of 200-300 ℃ below the gamma' phase solid solution temperature at the speed of 10-15 ℃/min, preserving the heat for 5-10 hours, and finally air-cooling to the room temperature;
the cast high-temperature alloy is Fe-Ni-based or Ni-based high-temperature alloy.
2. The overaging heat treatment process for cast superalloys of claim 1, wherein the cast superalloy has a γ' phase volume fraction of no less than 15% at thermodynamic equilibrium.
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| CN110760770B (en) * | 2019-10-30 | 2020-10-23 | 西安交通大学 | Heat treatment method for single crystal nickel-based high-temperature alloy after cold deformation |
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| CN105543568A (en) * | 2015-12-21 | 2016-05-04 | 杭州浙高合金材料有限公司 | Platinum-contained and rhenium-free nickel base single crystal superalloy and preparation method and application thereof |
| CN106756249A (en) * | 2016-12-09 | 2017-05-31 | 中国科学院金属研究所 | A kind of nickel-base high-temperature single crystal alloy of high intensity and tissue stabilization and preparation method thereof |
| CN106756253A (en) * | 2016-12-30 | 2017-05-31 | 江苏鑫信润科技有限公司 | Brush seal high-performance high-temperature nickel-base alloy brush filament material |
| CN106636759A (en) * | 2017-01-05 | 2017-05-10 | 中国科学院金属研究所 | Platinum group element reinforced high-thermal stability and high-strength nickel-based single-crystal high-temperature alloy |
| CN106834990A (en) * | 2017-01-19 | 2017-06-13 | 华能国际电力股份有限公司 | Heat treatment process for improving high-temperature tensile plasticity of nickel-iron-chromium-based wrought high-temperature alloy |
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