CN102418147A - High strength and completely antioxidative third generation monocrystalline high temperature alloy and preparation method thereof - Google Patents
High strength and completely antioxidative third generation monocrystalline high temperature alloy and preparation method thereof Download PDFInfo
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- CN102418147A CN102418147A CN2010102928223A CN201010292822A CN102418147A CN 102418147 A CN102418147 A CN 102418147A CN 2010102928223 A CN2010102928223 A CN 2010102928223A CN 201010292822 A CN201010292822 A CN 201010292822A CN 102418147 A CN102418147 A CN 102418147A
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Abstract
The invention relates to the field of high strength monocrystalline high temperature alloy and especially provides a high strength and completely antioxidative third generation monocrystalline high temperature alloy with low cost, and is mainly suitable for blade material of an aircraft engine used at a temperature higher than 1100 DEG C. The alloy comprises chemical components (wt%) of 3-5% of Cr, 5-12% of Co, 6-8% of W, 0.1-2% of Mo, 4.5-5.5% of Re, 5.5-7% of Al, 6-10% of Ta and the balance of Ni. The preparation method is as below: a monocrystalline blade or a testing rod is prepared at a monocrystalline growth furnace temperature gradient of 40K/cm-80K/cm, a cast temperature of 1480-1550 DEG C, with a shuttering temperature and a cast temperature kept at the same and a growth rate of 4-8mm/min; then, the alloy is treated with solid solution homogenizing treatment, high temperature aging treatment and low temperature aging treatment to gain high lasting intensity and creep limit. The alloy has a life no less than 200 h under a lasting condition of 1100 DEG C / 140 MPa and a lasting intensity similar to CMSX-10 and good high temperature antioxidative property, which is good surface stability Besides, a heat treatment window is wide, and the solid solution treatment is easy to control.
Description
Technical field
The present invention relates to HS single crystal super alloy and fields such as preparation and thermal treatment thereof; A kind of low cost, HS and complete oxidation resistant third generation single crystal super alloy are provided especially, mainly have been applicable to blade material in the aircraft engine of using more than 1100 ℃.
Background technology
Nickel-base high-temperature single crystal alloy is owing to have superior over-all properties, be at present and in the future quite over a long time in the advanced mover withstand temp the highest, the preferred material of the key part that stress-loaded is maximum.
In the process of single crystal super alloy development; Since to use temperature require increasingly high; The content of refractory element increases gradually in the alloy; Especially Re, W, Mo, Ta etc., the content of the typical first-generation (CMSX-2), the s-generation (CMSX-4), the third generation (CMSX-10) single crystal super alloy refractory element (Re+W+Mo+Ta) from about 14wt% near 16.5wt% again to above 20wt%.Especially, the Re content of CMSX-10 is 6wt%.Because the excessive adding of Re, W has also brought following shortcoming on the basis that performance is progressively improved: cost is high, density is big, microstructure is unstable, is prone to separate out TCP phase (topologically closepacked) etc.In order to solve the microstructure problem of unstable of second and third generation single crystal super alloy appearance; The external technique means that adopts is to add Ru, Ir and platinum family element to wait and suppress TCP and must separate out mutually, but these elements are more expensive than Re, and cost is higher; And resource shortage is difficult to a large amount of uses.In addition, the no Re alloy of domestic development, like DD99, DD98 etc., its performance is equivalent to the level of first, second monocrystalline in generation, and hot strength is low.The unique effect of Re is that Re gathers partially in the γ matrix, forms the Re atomic group of the about 1nm of size, hinders dislocation motion, can produce than the more tangible strengthening effect of single atom, adds the Re of 3wt%, can make temperature improve about 30 ℃.Re not only self spread coefficient is very low, can also reduce the bulk diffusion coefficient of other alloying element, all processes by diffusion control that can slow down, thereby the coarsening rate of the strengthening phase γ ' particle that slowed down, the velocity of diffusion of the control creep mechanism that also slowed down.So, obtain high hot strength, must add the Re element of certain content.
Summary of the invention
The purpose of this invention is to provide a kind of low cost, HS and complete oxidation resistant third generation single crystal super alloy, problems such as the cost height that exists in the solution prior art, microstructure instability, its use temperature can reach more than 1100 ℃.
Technical scheme of the present invention is:
According to the object of the invention, also consider simultaneously the effect of each alloying element, the content of Re is chosen for 4.5～5.5wt%, suitably improve the content of W and Ta simultaneously.HS of the present invention and complete oxidation resistant third generation single crystal super alloy, its concrete chemical ingredients (wt%) be as follows:
Cr3～5%, Co 5～12%, and W 6～8%, and Mo 0.1～2%, and Re 4.5～5.5%, and Al 5.5～7%, Ta6～10%, all the other are Ni.
HS of the present invention and complete oxidation resistant third generation single crystal super alloy, its preferred chemical ingredients (wt%) be as follows: Cr 3～4%, and Co 8～12%, and W 6～7%, and Mo 1～2%, and Re 4.5～5.0%, and Al 6～7%, and Ta 7～9%, and all the other are Ni.
HS of the present invention and complete oxidation resistant third generation single crystal super alloy, its best chemical ingredients (wt%) be as follows:
The preparation method of third generation single crystal alloy of the present invention:
On directional solidification furnace, prepare single crystal alloy; The temperature gradient of monocrystal growing furnace (directed stove) is between 40K/cm～80K/cm; Teeming temperature is 1480～1550 ℃; Mould shell temperature and teeming temperature are consistent, in growth velocity is 3～8mm/min scope, and preparation single crystal blade or coupon.
The heat treating regime of third generation single crystal alloy of the present invention is following:
(1) solution treatment was 1320～1330 ℃ of insulations 8～16 hours; Be warming up to 1335-1340 ℃ of insulation 8～16 hours subsequently, air cooling is to room temperature then;
(2) high-temperature aging is handled, and 1100～1150 ℃ of insulations 2～6 hours, air cooling was to room temperature subsequently;
(3) low temperature aging is handled, and 850～890 ℃ of insulations 16～26 hours, air cooling was to room temperature subsequently.
Principle of work of the present invention is following:
Though the design of the composition of alloy of the present invention has been chosen and has been lower than average Re content, through abundant solid solution, change aging temp and time, brings into play the solution strengthening of alloying element and the precipitation strength effect of γ ' as much as possible; Also utilize simultaneously the interaction of alloying element, make alloy reach the performance level of third generation monocrystalline with low Re content.
Design of chemical composition is mainly based on following reason:
Cr can improve the corrosion resistance of alloy, so the content of Cr must be enough big; Simultaneously, the content of Cr again should be as far as possible little, makes matrix can dissolve high-load Re, W, Mo etc. to obtain excellent creep property.In third generation single crystal super alloy, the content of Cr is generally 3～5wt%.
Co is very disputable to mutually sedimentary effect, Co ability stable alloy, but reduced breaking tenacity and oxidation-resistance.Erickson limits Co at 3wt% in CMSX-10, claim to do like this to have reduced the tendency that TCP forms mutually; Walston has recommended high-load Co Rene N6 (reaching 12.5wt%), in order to improve phase stability; Previous work of the present invention shows, the homogenizing of alloying constituent when Co helps thermal treatment, and the content of selected Co is at 5～12wt%.
Elements such as Al, Ti, Ta, Nb have determined the quantity of γ ' phase, and Nb strengthens γ ' phase, but harmful to the oxidation and the hot corrosion resistance of alloy, are prone to be combined into NbC with carbon; Ti is favourable to the corrosion resistance of alloy, but the reaction during to the castability of antioxidant property, alloy, solution heat treatment has negative impact, the 3rd, the 4th generation monocrystalline very low with the content control of Ti all, even remove fully.Ta improves the intensity of alloy through solution strengthening and raising γ ' particulate intensity; Ta is not the forming element of TCP phase; Ta can suppress the formation of freckle defective in the castingprocesses; Ta can improve the solvus of γ ' phase, and can promote the persistence of anti-oxidant, the hot corrosion resistance and the aluminum coating of alloy effectively.Therefore, remove Nb and Ti in the alloy of the present invention fully, the content of Ta is at 6～10wt%, and Al content is at 5.5～7wt%.
Mo is the solution strengthening element, and can increase the mismatch of γ/γ ', makes the misfit dislocation net intensive, can hinder dislocation motion effectively, and performance is improved; But Mo has very bad influence to the hot corrosion resistance of alloy, so the content of Mo is at 0.1～2wt%.
Re has significantly reduced the kinetic factor of γ ' phase grain growth alligatoring, and Re gathers partially in the γ matrix, forms elementide; Hinder dislocation motion; Ability produces than the more tangible strengthening effect of single atom, adds the Re of 3wt%, can make not hold when temperature ability force rate does not contain Re to improve about 30 ℃.Re can reduce the bulk diffusion coefficient of other element, all processes by diffusion control that can slow down, thereby the sedimentary coarsening rate of strengthening phase γ ' that slowed down, the velocity of diffusion of the control creep mechanism that also slowed down.Thereby the alloy that contains Re has great advantage at the high temperature tool, and the content of selected Re is at 4.5～5.5wt%.
W is strong solution strengthening element, under the situation of low Re content, give full play to the strengthening effect of W and Ta.But Re and W add the instability that excessive meeting causes microstructure, make the supersaturation of γ phase, are prone to form σ phase, μ phase, the equal TCP fragility phase of P.A spot of μ can not influence the mechanical property of alloy mutually; But the rupture life of alloy can sharply descend when the σ of rich Re precipitates increase mutually.And Re and W add excessive meeting and cause occurring in the alloy freckle that the chain equi-axed crystal is formed.Its reason is that solute segregation causes the main body liquid phase of the fluid density of mushy zone less than top, causes convective instability and causes secondary dendrite fracture.In alloy of the present invention, the content of W is at 6～8wt%.
The present invention adopts vacuum induction melting, is cast into mother alloy earlier, heat-treats according to aforesaid monocrystalline growing process and heat treating regime again.
The invention has the beneficial effects as follows:
1, the present invention adopts directional freeze to prepare single crystal alloy, handles and the low temperature aging processing through the processing of solid solution homogenizing, high-temperature aging, makes alloy of the present invention have high creep rupture strength and creeping limit.
2, compared with present technology, the present invention has higher medium and high temperature strength and good antioxidant property.
(1) instantaneous stretching performance
800℃：σ
0.2≥950MPa；1100℃：σ
0.2≥490MPa；
(2) enduring quality
1100 ℃/140MPa following creep rupture life >=200h; 1120 ℃/140MPa following creep rupture life >=100h, its creep rupture strength and CMSX-10 are suitable; High-temperature oxidation resistance is good, and promptly surface stability is good.
3, noble element Re content is low in the alloy of the present invention, thereby cost, density are low.
4, heat treatment window of the present invention is wide, and solution treatment is easy to control.
Description of drawings
Fig. 1 is the microtexture after the complete thermal treatment of embodiment alloy.
Fig. 2 is the Larson-Miller curve contrast of embodiment alloy and typical third generation single crystal alloy.
Fig. 3 (a)-(b) is the creep curve of embodiment alloy under differing temps and stress condition when creep compliance (certain abort).Creep curve when wherein, Fig. 3 (a) is 900 ℃ under the different stress; Creep curve when Fig. 3 (b) is 1000 ℃ under the different stress.
The relation of the overall strain width of cloth of low cycle fatigue and fracture cycle when Fig. 4 is 900 ℃ of embodiment alloys.
Fig. 5 is the constant temperature oxidation weight gain curve of embodiment alloy in the time of 1150 ℃.
Embodiment
Embodiment
The concrete composition of alloy of the present invention is seen table 1, in order to contrast conveniently, has also listed the chemical ingredients of CMSX-4 and CMSX-10 in the table 1.
The chemical ingredients of table 1 embodiment of the invention and comparative alloy CMSX-4 and CMSX-10 (wt%)
By said alloying constituent prepare burden with vacuum induction melting after, be cast into the master alloy ingot that is of a size of φ 80 * 500mm, the scale removal of polishing then is cut into suitable piece material and is used to prepare single crystal rod.
Single crystal rod adopts the spiral crystal separation method on directional solidification furnace, to prepare.Monocrystal growing furnace thermograde 60K/cm, 1550 ℃ of teeming temperatures, mould shell temperature and teeming temperature are consistent; After leaving standstill 10 minutes, use predetermined single crystal growth rate to carry out pull, prepare single crystal rod as 5mm/min.
Heat treating regime is following:
1330 ℃/16h+1340 ℃/16h (air cooling)+1150 ℃/4h (air cooling)+870 ℃/24h (air cooling); Adopt heat treating regime of the present invention can make eutectic and as cast condition γ ' dissolving more than 99%; The cubes γ ' that separates out uniform distribution and regularly arranged tiny (0.4～0.5 μ m) mutually; And make alloying constituent reach the ideal uniform distribution, help realizing the stable and strengthening effect of bringing into play Re to greatest extent of alloy structure.Microtexture after the complete thermal treatment of alloy is as shown in Figure 1.
Alloy is seen table 2 in the instantaneous stretching performance of differing temps.
The instantaneous stretching performance of table 2 embodiment alloy
Can find out that from table 2 between the room temperature to 800 ℃, the ys of alloy and tensile strength show increase to a certain degree with the rising of temperature; Especially the increase of tensile strength is more obvious; In the time of 800 ℃, reach intensity peak, after 800 ℃, intensity reduces fast; But the ys in the time of 1100 ℃ still reaches 490MPa, but knowledge capital invention alloy has higher medium and high temperature strength level.
The performance data of embodiment alloy under the lasting condition of difference is as shown in table 3, can find out, alloy has higher creep rupture life and rupture ductility, possesses the possibility of using more than 1100 ℃.
The enduring quality of table 3 embodiment alloy
| Lasting condition | Creep rupture life (h) | Unit elongation (%) |
| 1120℃/140MPa | 101.33 | 35.92 |
| 1120℃/140MPa | 106.42 | 43.52 |
| 1100℃/140MPa | 244.13 | 31.36 |
| 1100℃/140MPa | 257.87 | 51.52 |
| 1100℃/120MPa | 497 | 27.84 |
| 1100℃/170MPa | 96.17 | 39.04 |
| 1000℃/290MPa | 156.15 | 27.52 |
| 1000℃/260MPa | 257.68 | 24.16 |
| 1000℃/250MPa | 344.05 | 31.52 |
| 900℃/550MPa | 100.87 | 29.36 |
| 900℃/490MPa | 258.47 | 30.88 |
| 900℃/460MPa | 513.15 | 32.72 |
The Larson-Miller curve contrast of embodiment alloy and typical third generation single crystal alloy is as shown in Figure 2; Can find out; In very wide temperature and stress range; The invention alloy has identical enduring quality level with exemplary alloy, and alloy of the present invention has tangible low density, advantage cheaply, explains that alloy of the present invention has broad prospect for its application.
Fig. 3 (a)-(b) is the creep curve of embodiment alloy under differing temps and stress; Abort when each sample is creep compliance and reaches certain numerical value; Can find out except the condition of high ground stress of 900 ℃/390MPa; It is very low and continue very long state creep stage all to show creep speed under other condition, and promptly alloy has superior creep resistance.
The fracture cycle of the low cycle fatigue of embodiment alloy in the time of 900 ℃ and the relation of the overall strain width of cloth are as shown in Figure 4, and sample is smooth sample, and strain ratio is K
t=-1, waveform is a choppy sea.Can find out N
f=10
5The time the overall strain width of cloth be 0.5%, corresponding fatigue strength is 490MPa, shows that alloy has good fatigue resistance.
The constant temperature oxidation weight gain curve of embodiment alloy in the time of 1150 ℃ is as shown in Figure 5, and its average rate of oxidation is 0.786g/m
2H is anti-oxidant level, and the alloy that shows has good oxidation drag.
Claims (5)
1. HS and complete oxidation resistant third generation single crystal super alloy, it is characterized in that: by weight percentage, the chemical ingredients of this single crystal alloy is: Cr 3～5%; Co 5～12%, and W 6～8%, and Mo 0.1～2%; Re 4.5～5.5%; Al 5.5～7%, and Ta 6～10%, and all the other are Ni.
2. according to the described third generation single crystal super alloy of claim 1, it is characterized in that: by weight percentage, the preferred chemical ingredients of this single crystal alloy is following: Cr 3～4%; Co 8～12%, and W 6～7%, and Mo 1～2%; Re 4.5～5.0%; Al 6～7%, and Ta 7～9%, and all the other are Ni.
3. according to the described third generation single crystal super alloy of claim 1, it is characterized in that: by weight percentage, the best chemical ingredients (wt%) of this single crystal alloy as follows:
Cr 3%, and Co 12%, and W 6%, and Mo 1%, and Re 5%, and Al 6.2%, and Ta 8%, and all the other are Ni.
4. according to the preparation method of the described third generation single crystal super alloy of claim 1; It is characterized in that: on directional solidification furnace, prepare single crystal alloy; At monocrystal growing furnace temperature gradient 40K/cm～80K/cm, 1480～1550 ℃ of teeming temperatures, mould shell temperature and teeming temperature are consistent; In growth velocity is 3～8mm/min scope, preparation single crystal blade or coupon.
5. according to the preparation method of the described third generation single crystal super alloy of claim 4, it is characterized in that the heat treating regime of this single crystal alloy is following:
(1) solution treatment 1320～1330 ℃ of insulations 8～16 hours, is warming up to 1335-1340 ℃ of insulation 8～16 hours subsequently, and air cooling is to room temperature then;
(2) high-temperature aging is handled, and 1100～1150 ℃ of insulations 2～6 hours, air cooling was to room temperature subsequently;
(3) low temperature aging is handled, and 850～890 ℃ of insulations 16～26 hours, air cooling was to room temperature subsequently.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103382536A (en) * | 2012-05-03 | 2013-11-06 | 中国科学院金属研究所 | Fourth-generation single-crystal high temperature alloy with high strength and stable structure and preparation method thereof |
| CN103966671A (en) * | 2014-03-31 | 2014-08-06 | 中国科学院金属研究所 | High-strength hot-corrosion-resistant Ni-based single crystal superalloy and preparation method |
| 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 |
| CN109576532A (en) * | 2018-12-10 | 2019-04-05 | 中国科学院金属研究所 | Third generation single crystal super alloy and the preparation of creep rupture strength height and oxidation resistant |
| CN110846600A (en) * | 2019-10-30 | 2020-02-28 | 西安交通大学 | Multi-step reversion heat treatment method for additive manufacturing of single crystal nickel-based high-temperature alloy |
| CN111004944A (en) * | 2019-12-31 | 2020-04-14 | 长安大学 | High-molybdenum second-generation nickel-based single crystal superalloy and preparation method thereof |
| CN114250519A (en) * | 2022-01-10 | 2022-03-29 | 西北工业大学 | Solid solution heat treatment method for reducing content of solid solution holes of high-rhenium nickel-based single crystal superalloy |
| CN114737081A (en) * | 2022-04-06 | 2022-07-12 | 暨南大学 | Ni-Al-Ti-based high-temperature alloy with layered microstructure and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103382536A (en) * | 2012-05-03 | 2013-11-06 | 中国科学院金属研究所 | Fourth-generation single-crystal high temperature alloy with high strength and stable structure and preparation method thereof |
| CN103966671A (en) * | 2014-03-31 | 2014-08-06 | 中国科学院金属研究所 | High-strength hot-corrosion-resistant Ni-based single crystal superalloy and preparation method |
| 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 |
| CN109576532A (en) * | 2018-12-10 | 2019-04-05 | 中国科学院金属研究所 | Third generation single crystal super alloy and the preparation of creep rupture strength height and oxidation resistant |
| CN110846600A (en) * | 2019-10-30 | 2020-02-28 | 西安交通大学 | Multi-step reversion heat treatment method for additive manufacturing of single crystal nickel-based high-temperature alloy |
| CN111004944A (en) * | 2019-12-31 | 2020-04-14 | 长安大学 | High-molybdenum second-generation nickel-based single crystal superalloy and preparation method thereof |
| CN114250519A (en) * | 2022-01-10 | 2022-03-29 | 西北工业大学 | Solid solution heat treatment method for reducing content of solid solution holes of high-rhenium nickel-based single crystal superalloy |
| CN114737081A (en) * | 2022-04-06 | 2022-07-12 | 暨南大学 | Ni-Al-Ti-based high-temperature alloy with layered microstructure and preparation method thereof |
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Application publication date: 20120418 |