CN102071385A - Controlled directional solidification nickel-base high-temperature alloy recrystallizing method - Google Patents
Controlled directional solidification nickel-base high-temperature alloy recrystallizing method Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 74
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- 238000007711 solidification Methods 0.000 title claims abstract description 40
- 230000008023 solidification Effects 0.000 title claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 38
- 238000001953 recrystallisation Methods 0.000 claims abstract description 22
- 239000012086 standard solution Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 6
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- 239000010439 graphite Substances 0.000 claims abstract description 4
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
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Abstract
The invention provides a controlled directional solidification nickel-base high-temperature alloy recrystallizing method, which is characterized in that: a carburization and circulating heat treatment combined process is adopted to perform the heat treatment on a deformed directional solidification nickel-base high-temperature alloy, and then the alloy is subjected to standard solution treatment; a carburization is a micro-arc-spark carburization, the carburization material is a graphite electrode, and the carburization process parameters include a frequency of 1,000 to 5,000Hz, a power of 500 to 3,000W and a voltage of 20 to 100V; and the highest heat treatment temperature in each period of a circulating heat treatment process is at least 20 DEG C lower than the solid solution temperature of the alloy, the lowest heat treatment temperature in each period is not lower than the aging heat treatment of the alloy, and 3 to 10 circulation periods are adopted. The method can reduce the recrystallization-nucleation on the surface of the alloy, inhibit the growth of recrystals, reduce the stored energy of the deformed alloy, and thus control the recrystallization and obviously reduce the recrystals generated after the deformation of the nickel-base high-temperature alloy.
Description
Technical field
The present invention relates to the recrystallize control techniques, particularly a kind of carburizing is in conjunction with the technology that loops back re-heat treatment process control directional freeze column crystal or monocrystal nickel-base high-temperature alloy recrystallize.
Background technology
Internal combustion turbine, blade of aviation engine all are to use under comparatively high temps, and blade mainly is subjected to centrifugal action, and at high temperature, the intensity of crystal boundary is not as intracrystalline intensity, and laterally crystal boundary has just become the weak link of blade.For this reason, people have been developed directional columnargrain even single crystal blade and have been eliminated horizontal crystal boundary or whole crystal boundaries.Compare with traditional polycrystalline blade, these blades have the warm ability of holding of better vertical mechanical property and Geng Gao.
But blade is in the directional freeze process, because the difference of metal and ceramic-mould, core thermal expansivity, foundry goods can produce distortion.Also might produce distortion in shaping subsequently, sandblast, soldering even the military service process.Like this, vanes pyroprocessing (high temperature in solution treatment or the military service process) will produce recrystallize.Recrystallize produces horizontal crystal boundary, so formed the weak link of blade again, has a strong impact on the performance of blade.
At present, recrystallize for the generation of directional freeze blade, the measure of taking mainly is to control the distortion of blade (as reduce mechanical workout as far as possible, optimization design casting mold, core etc.) prevent blade to produce recrystallize, perhaps set up blade recrystallize standard, the strict detection, the blade that surpasses a certain degree recrystallize is scrapped at once.
Because blade unavoidably will pass through some operation (as sandblast etc.) in process of production, the distortion that these operations produced just can't be avoided.Therefore the recrystallize that brings can reduce casting qualified rate significantly, increases cost, has a strong impact on production efficiency.
For the control of recrystallize, some relevant reports are arranged abroad.European patent (patent No.: EP1038982 A1) adopt the method for gas (mainly being the mixed gas of CO and argon gas) carburizing that carbon is diffused into and form carbide in the alloy substrate, utilize carbide particle hinder crystal boundary migration be used for control recrystallize and recrystallize localized.The employed equipment of this method is complicated, operate more loaded down with trivial detailsly, and the cost height is controlled recrystallize with the method for control growing, and is mainly used in single crystal alloy.(patent No.: 5551999) adopt the regressive repeatedly method of lesser temps to control recrystallize, this method can not suppress recrystallize surface forming core and oxidation to United States Patent (USP).The method that adopts the coating the inside to add the grain-boundary strengthening element is in addition strengthened the recrystallize crystal boundary, avoid crackle to produce the (patent No.: EP 1036850A1), this method is primarily aimed at monocrystal nickel-base high-temperature alloy, and this method does not take in for the stress that brings in the coating procedure.What is more, and the method that adopts chemical corrosion is directly with the recrystallized layer erosion removal (patent No.: 5413648).Though it is this method can be removed recrystallized layer, obviously inapplicable for thin-walled monocrystalline or directional columnargrain nickel base superalloy parts.
Summary of the invention
The object of the invention provides a kind of control directional solidification nickel-base high-temperature alloy recrystallization method, reduce alloy surface recrystallize forming core by carburizing in conjunction with looping back the re-heat treatment process, suppressing recrystallize grows up, reduce the storage energy of deforming alloy, thereby the control recrystallize, the recrystallize that nickel base superalloy distortion back is produced significantly reduces.Special more remarkable for the control action kou of recrystallize that homogeneous deformation produces, the recrystallize that direct solid solution is produced with not passing through above-mentioned processing compares, and the recrystallize degree of depth reduces, and the recrystallize area occupied obviously reduces.
The present invention specifically provides a kind of control directional solidification nickel-base high-temperature alloy recrystallization method, it is characterized in that: adopt carburizing the directional solidification nickel-base high-temperature alloy that produces distortion to be heat-treated, then alloy is carried out the standard solution treatment in conjunction with looping back the re-heat treatment process;
Wherein carburization process is the micro-arc spark carburizing, and carburized material is a Graphite Electrodes, and carburizing process parameters is: frequency: 1000～5000HZ, power: 500～3000W, voltage: 20～100V;
The maximum heat treatment temperature that loops back each cycle of re-heat treatment process is than low 20 ℃ at least of the solid solubility temperatures of alloy, and the minimum thermal treatment temp in each cycle is not less than the timeliness thermal treatment temp of alloy, and loop cycle is 3～10 cycles.
The present invention utilizes the micro-arc spark carburization process that oneself directional solidification nickel-base high-temperature alloy of distortion is carried out carburizing treatment, then alloy is looped back re-heat and handles, and at last alloy is done the standard solution treatment.Because micro-arc spark carburizing covering alloy textured surface, can suppress alloy oxidation and recrystallize surface forming core on the one hand, the carbide particle of its generation can hinder recrystal grain and grows up on the other hand; Loop back the re-heat treatment process and can eliminate the unrelieved stress that carburizing brings, reduce the storage energy of deforming alloy, thereby reach the purpose of control recrystallize.
Control directional solidification nickel-base high-temperature alloy recrystallization method provided by the invention is characterized in that: described carburization process equipment used is micro-arc spark processing machine 3H-ES-1500.
Control directional solidification nickel-base high-temperature alloy recrystallization method provided by the invention is characterized in that: described carburization process frequency is 1000～2000HZ.
Control directional solidification nickel-base high-temperature alloy recrystallization method provided by the invention is characterized in that: described carburization process power is 1000～3000W.
Control directional solidification nickel-base high-temperature alloy recrystallization method provided by the invention is characterized in that: described carburization process voltage is 50～80V.
Suitable power, voltage and frequency can guarantee to obtain the cementation zone of appropriate depth, can also avoid damaging alloy substrate and over-drastic unrelieved stress.
Elimination directional solidification nickel-base high-temperature alloy recrystallization method provided by the invention is characterized in that; The described re-heat treatment process concrete steps that loop back are: slowly be warmed up to and loop back re-heat and handle starting temperature (T as shown in Figure 1
1), minimum thermal treatment temp T in start cycle
1Be the aging temp of alloy, maximum heat treatment temperature (T as shown in Figure 1
2) hanging down 100～150 ℃ than the solid solubility temperature of alloy, maximum heat treatment temperature and minimum thermal treatment temp increase by 20～30 ℃ successively in the cycle subsequently.
Control directional solidification nickel-base high-temperature alloy recrystallization method provided by the invention is characterized in that: described temperature rise rate and the rate of temperature fall that loops back between re-heat treatment process maximum heat treatment temperature and the minimum thermal treatment temp is 2～8 ℃/min.
Control directional solidification nickel-base high-temperature alloy recrystallization method provided by the invention is characterized in that: the described re-heat treatment process loop cycle that loops back is 3～6 cycles.Can guarantee like this to reach to reply effect preferably, again can be suitable enhance productivity.
Control directional solidification nickel-base high-temperature alloy recrystallization method provided by the invention is characterized in that: described looping back after the re-heat treatment process finishes, mode cold with stove or air cooling is cooled off.
Control directional solidification nickel-base high-temperature alloy recrystallization method provided by the invention, method has the following advantages: its carburization process is the micro-arc spark carburizing, and this processing unit is simple, the operation simple and feasible makes things convenient for manyly than gas cementation; Material therefor is a Graphite Electrodes, and with respect to CO and the argon gas that gas cementation is used, this material is drawn materials conveniently, and low price is convenient to deposit; Surperficial recrystallize forming core and alloy oxidation can be reduced in cementation zone covering alloy surface, and the second phase particle that carburizing forms hinders recrystallize and grows up; Loop back re-heat and handle the unrelieved stress that has reduced the carburization process introducing, consumed the storage energy of deforming alloy matrix, help reducing recrystallize.
Description of drawings
Fig. 1 loops back re-heat treatment process synoptic diagram;
Behind Fig. 2 sandblast distortion directional solidification nickel-base high-temperature alloy, the recrystallized structure that direct solution treatment is produced;
Behind Fig. 3 sandblast distortion directional solidification nickel-base high-temperature alloy, carburizing is passed through the recrystallized structure that solution treatment produced in conjunction with looping back after the re-heat treatment process is handled again.
Embodiment
Comparative example 1 carburizing control DZ125L directional solidificating alloy recrystallize.
Apparatus for directional solidification is prepared the directional solidification nickel-base high-temperature alloy plate, with the thin slice that cuts 3 * 12 * 12mm on the line cutting slave plate.With the face polishing of 12 * 12 (the directional columnargrain directions of growth), carry out carburizing treatment with the micro-arc spark processing machine.Carburization process equipment is micro-arc spark processing machine 3H-ES-1500, and micro-arc spark processing machine frequency is 1000HZ, and power is 1000W, and voltage is 50V.The carburizing treatment process will keep the even of surface cementation layer as far as possible.The water sand-blast device is done sandblasting then.The sandblast parameter is as follows: blasting pressure is 0.3MPa, and the sandblast time is 1min, and sand grains is SiO
2Glass sphere.
Sample is clean with alcohol wash, open heat treatment furnace, carry out the vacuum standard solution treatment, behind the air cooling sample is cut the recrystallized structure of observing generation.Through the sample of above-mentioned processing, the average recrystallize degree of depth is 18 microns, and the sample average recrystallize degree of depth of the direct solid solution of the above-mentioned processing of process is not 30 microns, the continuous and recrystallize degree of depth big (as shown in Figure 2) of recrystallize.
Embodiment 1 carburizing is in conjunction with looping back re-heat processing controls DZ125L directional solidification nickel-base high-temperature alloy recrystallize.
Apparatus for directional solidification is prepared the directional solidification nickel-base high-temperature alloy plate, with the square that cuts 3 * 12 * 12mm on the line cutting slave plate.With the face polishing of 12 * 12 (the directional columnargrain directions of growth), carry out carburizing treatment with the micro-arc spark processing machine.Carburization process equipment is micro-arc spark processing machine 3H-ES-1500, and micro-arc spark processing machine frequency is 1000HZ, and power is 1000W, and voltage is 50V.The carburizing treatment process will keep the even of surface cementation layer as far as possible.With sandblast apparatus sample is carried out sandblasting then.The sandblast parameter is as follows: blasting pressure is 0.3MPa, and the sandblast time is 1min, and sand grains is SiO
2Glass sphere.
Next open heat treatment furnace, set heat treatment process and be: room temperature is warmed up to 900 ℃ of time 90min, and 900 ℃ to 1100 ℃ 30min promptly guarantee the temperature rise rate of about 6 ℃/min, and 1100 ℃ to 920 ℃ 60min promptly guarantee the rate of temperature fall of about 3 ℃/min.In the ensuing cycle, corresponding temperature progressively improves 20-30 ℃, reach till 1190 ℃ up to top temperature, and when temperature arrives 900 ℃ once more, be 0 with time set, promptly stove is cold.Loop back in the re-heat treating processes, keep above-mentioned intensification and rate of temperature fall.After setting program thermal treatment, alloy sample is carried out the standard solution treatment, behind the air cooling alloy sample is cut, observe the recrystallized structure that produces.The sample recrystallize degree of depth through above-mentioned processing is 12 microns (Fig. 3), and the sample recrystallize degree of depth of the direct solution treatment of the above-mentioned processing of process is not 30 microns (Fig. 2).
Embodiment 2 carburizings are in conjunction with looping back re-heat processing controls DZ17G directional solidification nickel-base high-temperature alloy recrystallize.
Apparatus for directional solidification is prepared the directional solidification nickel-base high-temperature alloy plate, with the square that cuts 3 * 12 * 12mm on the line cutting slave plate.With the face polishing of 12 * 12 (the directional columnargrain directions of growth), carry out carburizing treatment with the micro-arc spark processing machine.Carburization process equipment is micro-arc spark processing machine 3H-ES-1500, and micro-arc spark processing machine frequency is 1000HZ, and power is 1000W, and voltage is 50V.The carburizing treatment process will keep the even of surface cementation layer as far as possible.With sandblast apparatus sample is carried out sandblasting then.The sandblast parameter is as follows: blasting pressure is 0.3MPa, and the sandblast time is 1min, and sand grains is SiO
2Glass sphere.
Next open heat treatment furnace, set heat treatment process and be: room temperature is warmed up to 900 ℃ of time 90min, and 900 ℃ to 1100 ℃ 30min promptly guarantee the temperature rise rate of about 6 ℃/min, and 1100 ℃ to 920 ℃ 60min promptly guarantee the rate of temperature fall of about 3 ℃/min.In the ensuing cycle, corresponding temperature progressively improves 20-30 ℃, reach till 1190 ℃ up to top temperature, and when temperature arrives 900 ℃ once more, be 0 with time set, promptly stove is cold.Loop back in the re-heat treating processes, keep above-mentioned intensification and rate of temperature fall.After setting program thermal treatment, alloy sample is carried out the standard solution treatment, behind the air cooling alloy sample is cut, observe the recrystallized structure that produces.The sample average recrystallize degree of depth through above-mentioned processing is 16 microns, and the sample average recrystallize degree of depth of the direct solution treatment of the above-mentioned processing of process is not 40 microns.
Embodiment 3 carburizings are in conjunction with looping back re-heat processing controls DZ125L directional solidification nickel-base high-temperature alloy recrystallize.
Apparatus for directional solidification is prepared the directional solidification nickel-base high-temperature alloy plate, with the square that cuts 3 * 12 * 12mm on the line cutting slave plate.With the face polishing of 12 * 12 (the directional columnargrain directions of growth), carry out carburizing treatment with the micro-arc spark processing machine.Carburization process equipment is micro-arc spark processing machine 3H-ES-1500, and micro-arc spark processing machine frequency is 1000HZ, and power is 2000W, and voltage is 50V.The carburizing treatment process will keep the even of surface cementation layer as far as possible.With sandblast apparatus sample is carried out sandblasting then.The sandblast parameter is as follows: blasting pressure is 0.3MPa, and the sandblast time is 1min, and sand grains is SiO
2Glass sphere.
Next open heat treatment furnace, set heat treatment process and be: room temperature is warmed up to 900 ℃ of time 90min, and 900 ℃ to 1100 ℃ 25min promptly guarantee the temperature rise rate of about 8 ℃/min, and 1100 ℃ to 920 ℃ 90min promptly guarantee the rate of temperature fall of about 2 ℃/min.In the ensuing cycle, corresponding temperature progressively improves 20-30 ℃, reach till 1190 ℃ up to top temperature, and when temperature arrives 900 ℃ once more, be 0 with time set, promptly stove is cold.Loop back in the re-heat treating processes, keep above-mentioned intensification and rate of temperature fall.After setting program thermal treatment, alloy sample is carried out the standard solution treatment, behind the air cooling alloy sample is cut, observe the recrystallized structure that produces.The sample recrystallize degree of depth through above-mentioned processing is 10 microns, and the sample recrystallize degree of depth of the direct solution treatment of the above-mentioned processing of process is not 30 microns (Fig. 2).
Claims (9)
1. a control directional solidification nickel-base high-temperature alloy recrystallization method is characterized in that: adopt carburizing in conjunction with looping back the re-heat treatment process directional solidification nickel-base high-temperature alloy that produces distortion to be heat-treated, then alloy is carried out the standard solution treatment;
Wherein carburization process is the micro-arc spark carburizing, and carburized material is a Graphite Electrodes, and carburizing process parameters is: frequency: 1000～5000HZ, power: 500～3000W, voltage: 20～100V;
The maximum heat treatment temperature that loops back each cycle of re-heat treatment process is than low 20 ℃ at least of the solid solubility temperatures of alloy, and the minimum thermal treatment temp in each cycle is not less than the timeliness thermal treatment temp of alloy, and loop cycle is 3～10 cycles.
2. according to the described control directional solidification nickel-base high-temperature alloy of claim 1 recrystallization method, it is characterized in that: described carburization process equipment used is micro-arc spark processing machine 3H-ES-1500.
3. according to the described control directional solidification nickel-base high-temperature alloy of claim 1 recrystallization method, it is characterized in that: described carburization process frequency is 1000～2000HZ.
4. according to the described control directional solidification nickel-base high-temperature alloy of claim 1 recrystallization method, it is characterized in that: described carburization process power is 1000～3000W.
5. according to the described control directional solidification nickel-base high-temperature alloy of claim 1 recrystallization method, it is characterized in that: described carburization process voltage is 50～80V.
6. according to the described control directional solidification nickel-base high-temperature alloy of claim 1 recrystallization method, it is characterized in that: described looping back in the re-heat treatment process, start cycle, minimum thermal treatment temp was the aging temp of alloy, maximum heat treatment temperature hangs down 100～150 ℃ than the solid solubility temperature of alloy, and maximum heat treatment temperature and minimum thermal treatment temp increase by 20～30 ℃ successively in the cycle subsequently.
7. according to the described control directional solidification nickel-base high-temperature alloy of claim 1 recrystallization method, it is characterized in that: described temperature rise rate and the rate of temperature fall that loops back between re-heat treatment process maximum heat treatment temperature and the minimum thermal treatment temp is 2～8 ℃/min.
8. according to the described control directional solidification nickel-base high-temperature alloy of claim 1 recrystallization method, it is characterized in that: the described re-heat treatment process loop cycle that loops back is 3～6 cycles.
9. according to the described control directional solidification nickel-base high-temperature alloy of claim 1 recrystallization method, it is characterized in that: described looping back after the re-heat treatment process finishes, mode cold with stove or air cooling is cooled off.
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| CN103668022A (en) * | 2013-12-13 | 2014-03-26 | 江苏大学 | Method for reducing inner residual stress of nickel-based superalloy |
| CN107119325A (en) * | 2017-06-26 | 2017-09-01 | 中国科学院金属研究所 | A kind of method for eliminating laser 3D printing single crystal super alloy recrystallization tendency |
| CN108193166A (en) * | 2016-12-08 | 2018-06-22 | 沈阳金研激光再制造技术开发有限公司 | Titanium alloy surface micro-arc carburization method |
| CN109724556A (en) * | 2017-10-27 | 2019-05-07 | 中国科学院金属研究所 | The recrystallization tendentiousness evaluation method of nickel-base high-temperature single crystal alloy hot investment casting process |
| CN110760769A (en) * | 2019-10-30 | 2020-02-07 | 西安交通大学 | Cold deformation recovery method for single crystal nickel-based superalloy |
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| CN115354133A (en) * | 2022-08-16 | 2022-11-18 | 中国航发北京航空材料研究院 | Method for preventing local recrystallization of single crystal superalloy blade |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5551999A (en) * | 1984-04-23 | 1996-09-03 | United Technologies Corporation | Cyclic recovery heat treatment |
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| CN103668022A (en) * | 2013-12-13 | 2014-03-26 | 江苏大学 | Method for reducing inner residual stress of nickel-based superalloy |
| CN108193166A (en) * | 2016-12-08 | 2018-06-22 | 沈阳金研激光再制造技术开发有限公司 | Titanium alloy surface micro-arc carburization method |
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| CN109724556B (en) * | 2017-10-27 | 2020-08-21 | 中国科学院金属研究所 | Method for evaluating recrystallization tendency in precision casting process of nickel-based single crystal superalloy |
| CN109724556A (en) * | 2017-10-27 | 2019-05-07 | 中国科学院金属研究所 | The recrystallization tendentiousness evaluation method of nickel-base high-temperature single crystal alloy hot investment casting process |
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| CN111593399A (en) * | 2020-05-22 | 2020-08-28 | 深圳市万泽航空科技有限责任公司 | Method for controlling recrystallization of single crystal high-temperature alloy |
| CN115094360A (en) * | 2022-07-13 | 2022-09-23 | 北航（四川）西部国际创新港科技有限公司 | Heat treatment process of single crystal high temperature alloy with deformation and recrystallization resistant effects |
| CN115094360B (en) * | 2022-07-13 | 2022-11-29 | 北航（四川）西部国际创新港科技有限公司 | Heat treatment process of single crystal high temperature alloy with deformation resistance and recrystallization resistance effects |
| CN115354133A (en) * | 2022-08-16 | 2022-11-18 | 中国航发北京航空材料研究院 | Method for preventing local recrystallization of single crystal superalloy blade |
| CN115354133B (en) * | 2022-08-16 | 2023-10-17 | 中国航发北京航空材料研究院 | Method for preventing local recrystallization of monocrystalline superalloy blade |
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