CN103382536A - Fourth-generation single-crystal high temperature alloy with high strength and stable structure and preparation method thereof - Google Patents
Fourth-generation single-crystal high temperature alloy with high strength and stable structure and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of high-strength single-crystal high temperature alloys and especially provides a fourth-generation single-crystal high temperature alloy with high strength and a stable structure and a preparation method thereof. The alloy is mainly applicable to aero-engine blade materials used at a temperature higher than 1100 DEG C. Chemical components of the alloy comprise, by weight, 3 to 5% of Cr, 5 to 12% of Co, 6 to 8% of W, 0.1 to 2% of Mo, 4.5 to 6% of Re, 2 to 4% of Ru, 5.5 to 6.5% of Al and 6 to 10% of Ta, with the balance being Ni. The preparation method comprises the following steps: preparing a single-crystal blade or test rod under the conditions that temperature gradient of a single crystal growth furnace is in a range of 40 K/cm to 80 K/cm, casting temperature is 1480 to 1550 DEG C, shuttering temperature is consistent with the casting temperature and a growth rate is 4 to 8 mm/min; and then carrying out solid solution homogenization treatment, high temperature aging treatment and low temperature aging treatment so as to allow the alloy provided by the invention to have high endurance strength. The alloy has a life of no less than 100 h in endurance conditions of a temperature of 1140 DEG C and a pressure of 137 MPa and has endurance strength equivalent to the endurance strength of an EPM102 alloy; and the alloy has the advantages of good structure stability at a high temperature, a wide heat treatment window and easily controllable solid solution treatment.
Description
Technical field
The invention belongs to high strength single crystal super alloy and the fields such as preparation and thermal treatment thereof, provide especially a kind of low cost, high strength and fully oxidation resistant the 4th generation single crystal super alloy, mainly be applicable to the blade material in the aircraft engine of using more than 1100 ℃.
Background technology
Nickel-base high-temperature single crystal alloy is owing to having superior over-all properties, be at present and in the future quite over a long time in advanced engine withstand temp the highest, the preferred material of the key part of stress-loaded maximum.
In the process of single crystal super alloy development, because the requirement to use temperature is more and more higher, in alloy, the content of refractory element increases gradually, 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 surpassing 20wt%.Especially, the Re content of CMSX-10 is 6wt%.Because the excessive of Re, W adds, also brought following shortcoming on the basis that performance is progressively improved: cost is high, density is large, microstructure is unstable, easily separates out TCP phase (topologically close packed) etc.In order to solve the unsettled problem of microstructure 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 etc. to suppress TCP must separate out mutually, the exemplary alloy of having developed comprises TMS-138, MC-NG and EPM102, these interpolation elements are even more expensive than Re simultaneously, cause cost of alloy further to raise.In addition, domestic development without the Re alloy, as DD99, DD98 etc., its performance is equivalent to the level of first, second monocrystalline in generation, hot strength is low.Re not only self spread coefficient is very low, can also reduce the bulk diffusion coefficient of other alloying element, and all processes by diffusion control that can slow down, thereby the coarsening rate of the strengthening phase γ ' particle that slowed down have also slowed down and controlled the velocity of diffusion of creep mechanism.The Re that adds 3wt% can make alloy hold warm ability and improve about 30 ℃.But the main segregation of Re and is difficult to eliminate fully dendritic segregation because velocity of diffusion is extremely low in matrix, therefore, the tendency of separating out the TCP phase increases the weight of.So, obtain high hot strength and good structure stability, the content of Re, Ru element be must optimize and best Re, Ru constituent content proportioning determined.
Summary of the invention
The objective of the invention is to solve the problems such as the cost that exists in prior art is high, microstructure is unstable, its use temperature can reach more than 1100 ℃, a kind of high strength is provided and organize stable the 4th generation single crystal super alloy and preparation method,,
The invention provides a kind of high strength and organize stable the 4th generation single crystal super alloy, by weight percentage, the chemical composition of this alloy is: Cr 3～5%, and Co 5～12%, and W 6～8%, Mo0.1～2%, Re 4.5～6%, and Ru 2～4%, and Al 5.5～6.5%, Ta 6～10%, and all the other are Ni.
High strength provided by the invention and organize stable the 4th generation single crystal super alloy, by weight percentage, the chemical composition of this alloy is preferably as follows: Cr 3.5～4.5%, and Co 8～12%, and W 6～7%, Mo 1～2%, Re 4.5～5.5%, and Ru 2.5～3.5%, and Al 5.75～6.25%, Ta 7～9%, and all the other are Ni.
High strength provided by the invention and organize stable the 4th generation single crystal super alloy, by weight percentage, chemical composition the best of this alloy is as follows: Cr 4%, Co 12%, W 6%, and Mo 1%, and Re 5.4%, and Ru 3%, Al 6%, and Ta 8.4%, and all the other are Ni.
The present invention described high strength also is provided and organize stable the 4th generation single crystal super alloy the preparation method, described alloying constituent is prepared single crystal alloy on directional solidification furnace according to proportioning, 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 was 3～8mm/min scope, then preparation single crystal blade or coupon heat-treated.
High strength provided by the invention and organize stable the 4th generation single crystal super alloy the preparation method, described heat treating regime is as follows:
(1) solution treatment: 1310～1320 ℃ of insulations 8～16 hours, be warming up to subsequently 1320-1330 ℃ of insulation 8～16 hours, then air cooling is to room temperature;
(2) high-temperature aging is processed: 1100～1150 ℃ of insulations 2～6 hours, air cooling was to room temperature subsequently;
(3) low temperature aging is processed: 850～890 ℃ of insulations 16～26 hours, air cooling was to room temperature subsequently.
Principle of work of the present invention is as follows:
Although the Composition Design of alloy of the present invention has been chosen lower than average Re content, by abundant solid solution, change aging temp and time, bring into play as much as possible the solution strengthening of alloying element and the precipitation strength effect of γ '; Also utilize simultaneously the interaction of alloying element, make the alloy with low Re content reach the 4th generation monocrystalline performance level.
The design of chemical composition is mainly based on following reason:
Cr can carry heavy alloyed corrosion resistance, so the content of Cr must be enough large; Simultaneously, the content of Cr again should be as far as possible little, makes matrix can dissolve Re, W, the Mo etc. of high-content to obtain excellent creep property.In the 4th generation single crystal super alloy, the content of Cr is generally 3～5wt%.
Co is very disputable to the effect that precipitates mutually, Co energy 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 the Co of high-content to reach 12.5wt% at Rene N6(), in order to improve phase stability; Previous work of the present invention shows, the homogenizing of alloying constituent when Co is conducive to thermal treatment, and the content of selected Co is at 5～12wt%.
The elements such as Al, Ti, Ta, Nb have determined the quantity of γ ' phase, and Nb strengthens γ ' phase, but the oxidation of alloy and hot corrosion resistance are harmful, and easy and carbon is combined into NbC; The corrosion resistance of Ti alloy is favourable, but the reaction during to the castability of antioxidant property, alloy, solution heat treatment has negative impact, the 3rd, the 4th generation monocrystalline all the content of Ti is controlled very low, remove even fully.Ta puies forward heavy alloyed intensity by the intensity of solution strengthening and raising γ ' particle, Ta is not the forming element of TCP phase, Ta can suppress the formation of freckle defective in castingprocesses, Ta can improve the solvus of γ ' phase, and can effectively promote the persistence of anti-oxidant, hot corrosion resistance and the aluminum coating of alloy.Therefore, remove Nb and Ti in alloy of the present invention fully, the content of Ta is at 6～10wt%, and Al content is at 5.5～6.5wt%.
Mo is the solution strengthening element, and can increase the mismatch of γ/γ ', makes the misfit dislocation net intensive, can effectively hinder dislocation motion, and performance is improved; But the hot corrosion resistance of Mo alloy has very bad impact, so the content of Mo is at 0.1～2wt%.
Re has significantly reduced the kinetic factor of γ ' phase grain growth alligatoring, and the Re segregation forms elementide in the γ matrix, hinder dislocation motion, can produce than the more obvious strengthening effect of single atom, add the Re of 3wt%, can make not hold when temperature energy force rate does not contain Re and improve about 30 ℃.Re can reduce the bulk diffusion coefficient of other element, and all processes by diffusion control that can slow down, thereby the coarsening rate of the strengthening phase γ ' precipitation that slowed down have also slowed down and controlled the velocity of diffusion of creep mechanism.Thereby the alloy that contains Re has great advantage at the high temperature tool, and the content of selected Re is at 4.5～6wt%.
Thereby the vital role of Ru is to suppress separating out of TCP phase to put forward heavy alloyed structure stability.About there being very large dispute in the microscopic mechanism document of Ru stabilizing tissue, a kind of viewpoint think Ru impel part Re from matrix γ phase transition to γ ' mutually, namely reduce the segregation of Re in matrix, thereby suppressed separating out of TCP phase by the negative segregation effect.Another kind of viewpoint thinks that thereby Ru itself has the effect that increases the solubleness of Re in matrix and reduces TCP phase proneness.Although to the mechanism of action of the Ru understanding of not yet agreeing, the effect of Ru stabilizing tissue has obtained admitting widely.In addition, the price of Ru itself is also very expensive, and Ru has the detrimental action of reduction γ ' phased soln temperature.Therefore, satisfying the content that reduces as far as possible Ru under the prerequisite that suppresses the TCP phase, the content of selected Ru is at 2～4wt%.
W is strong solution strengthening element, in the situation that low Re content will be given full play to the strengthening effect of W and Ta.But Re and W add excessive meeting to cause the unstable of microstructure, make the supersaturation of γ phase, easily form σ phase, μ phase, the equal TCP fragility phase of P.A small amount of μ can not affect 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 to cause occurring in alloy the freckle that the chain equi-axed crystal forms.Its reason is that solute segregation causes the fluid density of mushy zone less than the main body liquid phase on 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, first is cast into mother alloy, then prepares the monocrystalline coupon according to aforesaid monocrystalline growing process and heat treating regime.
The invention has the beneficial effects as follows:
1, the present invention adopts directional freeze to prepare single crystal alloy, processes 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 good structure stability.
2, compared with the prior art, the present invention has higher medium and high temperature strength.
(1) instantaneous stretching performance
800℃：σ
0.2≥895MPa；1000℃：σ
0.2≥580MPa；
(2) enduring quality
1100 ℃/180MPa lower creep rupture life 〉=80h; 1140 ℃/137MPa lower creep rupture life 〉=100h, its creep rupture strength and EPM102 alloy phase are worked as.
3, noble element Re in alloy of the present invention, Ru content are low, thereby cost is lower.
4, alloy solid solution temperature of the present invention is low, and heat treatment process is easy to implement.
Description of drawings
Fig. 1 is the microtexture after the embodiment 1 complete thermal treatment of alloy;
Fig. 2 is the Larson-Miller curve comparison of embodiment 1 alloy and typical case's the 4th generation single crystal alloy;
Fig. 3 is the microtexture of embodiment 1 alloy after 1100 ℃ of timeliness 1000h;
Fig. 4 is the microtexture after the embodiment 2 complete thermal treatments of alloy;
Fig. 5 is the Larson-Miller curve comparison of embodiment 2 alloys and typical case's the 4th generation single crystal alloy;
Fig. 6 is the microtextures of embodiment 2 alloys after 1100 ℃ of timeliness 1000h.
Embodiment
Following examples will be further described the present invention, but not thereby limiting the invention.
Embodiment 1
The concrete composition of alloy of the present invention sees Table 1, in order to contrast conveniently, has also listed the chemical composition of CMSX-4 and CMSX-10 in table 1.
The chemical composition of table 1 the present embodiment and comparative alloy CMSX-10 and EPM102 (wt%)
By described alloying constituent prepare burden and vacuum induction melting after, be cast into the master alloy ingot that is of a size of φ 80 * 500mm, the scale removal of then polishing is cut into suitable piece material for the preparation of single crystal rod.
Single crystal rod adopts the spiral crystal separation method to be prepared on directional solidification furnace.Monocrystal growing furnace thermograde 60K/cm, 1550 ℃ of teeming temperatures, mould shell temperature and teeming temperature are consistent; After standing 10 minutes, be that 5mm/min carries out pull with predetermined single crystal growth rate, prepare single crystal rod.
Heat treating regime is as follows:
1320 ℃/8h+1330 ℃/the 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%, separate out the cubes γ ' of even distribution and regularly arranged tiny (0.4～0.5 μ m) mutually, and make alloying constituent reach desirable even distribution, be conducive to realize the stable of alloy structure and bring into play to greatest extent the strengthening effect of Re.Microtexture after the complete thermal treatment of alloy as shown in Figure 1.
Alloy sees Table 2 in the instantaneous stretching performance of differing temps.
The instantaneous stretching performance of table 2 the present embodiment alloy
| Temperature (℃) | Yield strength (MPa) | Tensile strength (MPa) |
| 20 | 980 | 1090 |
| 760 | 955 | 1370 |
| 800 | 895 | 1150 |
| 1000 | 580 | 680 |
As can be seen from Table 2, between room temperature to 760 ℃, the yield strength of alloy is substantially constant, and tensile strength increases significantly with the rising of temperature, reaches intensity peak in the time of 760 ℃.After surpassing 760 ℃, the intensity fast reducing, but the yield strength 1000 ℃ the time still reaches 580MPa, and alloy of the present invention has higher medium and high temperature strength level as can be known.
The performance data of the present 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 the present embodiment alloy
The present embodiment alloy with typical case the 4th generation single crystal alloy the Larson-Miller curve comparison 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.
The microtexture of the present embodiment alloy after 1100 ℃ of Long-term Aging 1000h only separated out a small amount of corynebacterium and particulate state TCP mutually as shown in Figure 3 in visible alloy, show that alloy has good structure stability.
Embodiment 2
Be with the difference of embodiment 1, the composition of the present embodiment alloy sees Table 4, for ease of contrast, the composition of embodiment 1 is also listed in table.
By described alloying constituent prepare burden and vacuum induction melting after, be cast into the master alloy ingot that is of a size of φ 80 * 500mm, the scale removal of then polishing is cut into suitable piece material for the preparation of single crystal rod.
Single crystal rod adopts the spiral crystal separation method to be prepared on directional solidification furnace.Monocrystal growing furnace thermograde 60K/cm, 1550 ℃ of teeming temperatures, mould shell temperature and teeming temperature are consistent; After standing 10 minutes, be that 5mm/min carries out pull with predetermined single crystal growth rate, prepare single crystal rod.
Table 4 the present embodiment and embodiment 1 and EPM102 alloy composition (wt%)
Heat treating regime is as follows:
1317 ℃/8h+1327 ℃/the 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%, separate out the cubes γ ' of even distribution and regularly arranged tiny (0.4～0.5 μ m) mutually, and make alloying constituent reach desirable even distribution, be conducive to realize the stable of alloy structure and bring into play to greatest extent the strengthening effect of Re.Microtexture after the complete thermal treatment of alloy as shown in Figure 4.
The performance data of the present embodiment alloy under the lasting condition of difference is as shown in table 5, 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 5 the present embodiment alloy
The present embodiment alloy with typical case the 4th generation single crystal alloy the Larson-Miller curve comparison as shown in Figure 5, can find out, in very wide temperature and stress range, the invention alloy has identical enduring quality level with exemplary alloy.
The microtexture of the present embodiment alloy after 1100 ℃ of Long-term Aging 1000h as shown in Figure 6, γ ' in alloy is the raft shape tissue of formation rule, but the particulate state of only having minute quantity and corynebacterium TCP are mutually, show that alloy has good structure stability, at high temperature life-time service.
Above embodiment shows that alloy of the present invention has low density, advantage cheaply, illustrates that alloy of the present invention has wide popularizing application prospect.
Claims (5)
- A high strength and organize stable the 4th generation single crystal super alloy, it is characterized in that: by weight percentage, the chemical composition of this alloy is: Cr 3～5%, and Co 5～12%, and W 6～8%, Mo 0.1～2%, Re 4.5～6%, and Ru 2～4%, and Al 5.5～6.5%, Ta 6～10%, and all the other are Ni.
- According to the described high strength of claim 1 and organize stable the 4th generation single crystal super alloy, it is characterized in that: by weight percentage, the chemical composition of this alloy is as follows: Cr 3.5～4.5%, and Co 8～12%, and W 6～7%, Mo 1～2%, Re 4.5～5.5%, and Ru 2.5～3.5%, and Al 5.75～6.25%, Ta 7～9%, and all the other are Ni.
- According to the described high strength of claim 1-2 and organize stable the 4th generation single crystal super alloy, it is characterized in that: by weight percentage, the chemical composition of this alloy is as follows: Cr 4%, and Co 12%, W 6%, and Mo 1%, and Re 5.4%, and Ru 3%, Al 6%, and Ta 8.4%, and all the other are Ni.
- The described high strength of claim 1 and organize stable the 4th generation single crystal super alloy the preparation method, it is characterized in that: described alloying constituent is prepared single crystal alloy according to proportioning on directional solidification furnace, 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 was 3～8mm/min scope, then preparation single crystal blade or coupon heat-treated.
- According to the described high strength of claim 4 and organize stable the 4th generation single crystal super alloy the preparation method, it is characterized in that: described heat treating regime is as follows:(1) solution treatment: 1310～1320 ℃ of insulations 8～16 hours, be warming up to subsequently 1320-1330 ℃ of insulation 8～16 hours, then air cooling is to room temperature;(2) high-temperature aging is processed: 1100～1150 ℃ of insulations 2～6 hours, air cooling was to room temperature subsequently;(3) low temperature aging is processed: 850～890 ℃ of insulations 16～26 hours, air cooling was to room temperature subsequently.
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| CN109014215A (en) * | 2018-07-18 | 2018-12-18 | 西安交通大学 | A kind of heat treatment method of increasing material manufacturing monocrystal nickel-base high-temperature alloy |
| CN109338452A (en) * | 2018-12-06 | 2019-02-15 | 重庆科技学院 | A kind of method that heat treating process prepares large scale magnesium or magnesium alloy monocrystalline |
| CN115029586A (en) * | 2022-04-22 | 2022-09-09 | 中国科学院金属研究所 | Nickel-based single crystal superalloy and preparation method thereof |
| CN115029586B (en) * | 2022-04-22 | 2023-08-15 | 中国科学院金属研究所 | Nickel-based single crystal superalloy and preparation method thereof |
| CN115255336A (en) * | 2022-08-30 | 2022-11-01 | 北京航空航天大学 | Composite component single crystal thin-wall component and preparation method thereof |
| CN115255336B (en) * | 2022-08-30 | 2024-03-26 | 北京航空航天大学 | Composite component monocrystalline thin-wall component and preparation method thereof |
| CN115491620A (en) * | 2022-09-14 | 2022-12-20 | 浙江大学 | Under-aging heat treatment process for nickel-based wrought superalloy |
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Application publication date: 20131106 |