CN110241331B - Nickel-based powder superalloy and its preparation method and application - Google Patents
Nickel-based powder superalloy and its preparation method and application Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 166
- 239000000843 powder Substances 0.000 title claims abstract description 102
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 90
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 17
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 14
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 14
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 14
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 14
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 14
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 13
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 7
- 229910052762 osmium Inorganic materials 0.000 claims abstract description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 51
- 239000000956 alloy Substances 0.000 claims description 51
- 238000010438 heat treatment Methods 0.000 claims description 32
- 230000032683 aging Effects 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 18
- 239000011159 matrix material Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 10
- 238000004090 dissolution Methods 0.000 claims description 8
- 238000001513 hot isostatic pressing Methods 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000003466 welding Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- 238000009849 vacuum degassing Methods 0.000 claims description 4
- 238000010308 vacuum induction melting process Methods 0.000 claims description 4
- 241001062472 Stokellia anisodon Species 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000007780 powder milling Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 11
- 238000005728 strengthening Methods 0.000 description 9
- 238000005204 segregation Methods 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 5
- 210000001787 dendrite Anatomy 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- 229910052702 rhenium Inorganic materials 0.000 description 3
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
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- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910021472 group 8 element Inorganic materials 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 208000010125 myocardial infarction Diseases 0.000 description 1
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- 230000002085 persistent effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0433—Nickel- or cobalt-based alloys
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- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract
Description
技术领域technical field
本发明涉及粉末高温合金领域，具体而言，涉及镍基粉末高温合金及其制备方法与应用。The invention relates to the field of powder superalloy, in particular, to a nickel-based powder superalloy and a preparation method and application thereof.
背景技术Background technique
涡轮盘是航空发动机中最重要的热端部件之一，其在服役过程中，轮毂承受极大的离心力，需要较高的拉伸强度，而轮缘的温度比轮毂温度高，需要良好的高温持久性能和抗蠕变性能。航空发动机涡轮盘对材料的要求十分苛刻，不仅要求涡轮盘合金具有高拉伸强度、高损伤容限、高蠕变性能、高热疲劳性能，以及优异的抗氧化和耐腐蚀性等，而且要求涡轮盘合金在长时服役过程中拓扑密排(TCP)相析出倾向很小，使合金具有良好的高温组织稳定性，以保证合金力学性能的衰减降低到最低。Turbine disc is one of the most important hot-end components in aero-engines. During its service, the hub is subjected to great centrifugal force and requires high tensile strength. The temperature of the rim is higher than that of the hub, which requires good high temperature. Durability and creep resistance. Aero-engine turbine disks have very stringent requirements on materials, not only requiring turbine disk alloys with high tensile strength, high damage tolerance, high creep properties, high thermal fatigue properties, and excellent oxidation and corrosion resistance, but also requiring turbine disks. The precipitation tendency of topologically close-packed (TCP) phase of the disk alloy is very small during the long-term service, which makes the alloy have good high temperature microstructure stability, so as to ensure that the attenuation of the mechanical properties of the alloy is reduced to a minimum.
随着航空发动机的发展，涡轮盘的工作温度越来越高，目前新开发、研制的航空发动机要求涡轮盘的工作温度要达到815℃。而现有的用于涡轮盘的镍基粉末高温合金，如FGH4095、FGH4096、FGH4097、FGH4098等合金，它们的最高使用温度限制在650℃～750℃，超过750℃则会出现严重的TCP相，这些合金均无法满足在815℃高温下保持持久高性能的要求。With the development of aero-engines, the working temperature of the turbine disk is getting higher and higher. At present, the newly developed and developed aero-engine requires the working temperature of the turbine disk to reach 815 °C. However, the existing nickel-based powder superalloys for turbine disks, such as FGH4095, FGH4096, FGH4097, FGH4098 and other alloys, their maximum operating temperature is limited to 650 ° C ~ 750 ° C, and if the temperature exceeds 750 ° C, a serious TCP phase will appear. None of these alloys can meet the long-lasting high performance requirements at 815°C.
有鉴于此，特提出本发明。In view of this, the present invention is proposed.
发明内容SUMMARY OF THE INVENTION
本发明的第一目的在于提供一种镍基粉末高温合金，其具有优异综合性能的成分构成及含量赋予了所述镍基粉末高温合金优异的高温抗拉强度、屈服强度和高温持久性能以及更高的最高工作温度。The first object of the present invention is to provide a nickel-based powder superalloy, the composition and content of which have excellent comprehensive properties endow the nickel-based powder superalloy with excellent high-temperature tensile strength, yield strength, high-temperature durability and more High maximum operating temperature.
本发明的第二目的在于提供上述镍基粉末高温合金的制备方法，所述方法高效易行、重现性好，制备得到的镍基粉末高温合金显微组织结构稳定性高。The second object of the present invention is to provide a method for preparing the above-mentioned nickel-based powder superalloy, which is efficient, easy to implement, and has good reproducibility, and the prepared nickel-based powder superalloy has high microstructure stability.
本发明的第三目的在于提供应用了上述镍基粉末高温合金的航空设备。The third object of the present invention is to provide aviation equipment to which the above-mentioned nickel-based powder superalloy is applied.
为了实现本发明的上述目的，特采用以下技术方案：In order to realize the above-mentioned purpose of the present invention, the following technical solutions are specially adopted:
按质量分数计，所述镍基粉末高温合金的成分包括：In terms of mass fraction, the composition of the nickel-based powder superalloy includes:
C 0.02％～0.10％、Co 14.0％～22.0％、Cr 6.0％～14.0％、Mo 1.8％～4.0％、W3.0％～6.0％、Ta 2.5％～6.0％、Al 2.8％～4.0％、Ti 2.6％～4.4％、Nb 1.2％～3.2％、Hf 0.1％～0.5％、Zr 0.01％～0.08％、B 0.01％～0.08％、Os0.3％～6.0％和/或Ru0.5％～6.0％，以及余量的Ni；C 0.02% to 0.10%, Co 14.0% to 22.0%, Cr 6.0% to 14.0%, Mo 1.8% to 4.0%, W3.0% to 6.0%, Ta 2.5% to 6.0%, Al 2.8% to 4.0%, Ti 2.6%～4.4%, Nb 1.2%～3.2%, Hf 0.1%～0.5%, Zr 0.01%～0.08%, B 0.01%～0.08%, Os0.3%～6.0% and/or Ru0.5%～ 6.0%, and the balance of Ni;
所述镍基粉末高温合金中Al、Ti、Nb、Ta、Hf的总质量分数为12.5％～15.5％。The total mass fraction of Al, Ti, Nb, Ta and Hf in the nickel-based powder superalloy is 12.5% to 15.5%.
可选地，按质量分数计，所述镍基粉末高温合金的成分包括：Optionally, in terms of mass fraction, the composition of the nickel-based powder superalloy includes:
C 0.03％～0.08％、Co 15.0％～20.0％、Cr 7.0％～13.0％、Mo 2.6％～3.8％、W3.2％～5.5％、Ta 2.6％～3.8％、Al 3.0％～4.0％、Ti 2.8％～4.2％、Nb 1.4％～3.0％、Hf 0.15％～0.45％、Zr 0.01％～0.06％、B 0.01％～0.06％、Os 0.3％～3.0％和/或Ru0.5％～3.0％，以及余量的Ni。C 0.03%～0.08%, Co 15.0%～20.0%, Cr 7.0%～13.0%, Mo 2.6%～3.8%, W3.2%～5.5%, Ta 2.6%～3.8%, Al 3.0%～4.0%, Ti 2.8%～4.2%, Nb 1.4%～3.0%, Hf 0.15%～0.45%, Zr 0.01%～0.06%, B 0.01%～0.06%, Os 0.3%～3.0% and/or Ru0.5%～3.0 %, and the balance of Ni.
可选地，按质量分数计，所述镍基粉末高温合金的成分包括：Optionally, in terms of mass fraction, the composition of the nickel-based powder superalloy includes:
C 0.04％～0.07％、Co 16.0％～19.0％、Cr 8.0％～12.0％、Mo 2.7％～3.6％、W3.4％～5.0％、Ta 2.8％～3.6％、Al 3.1％～4.0％、Ti 3.0％～4.0％、Nb 1.6％～2.8％、Hf 0.2％～0.4％、Zr 0.01％～0.06％、B 0.01％～0.06％、Os 0.3％～3.0％和/或Ru0.5％～3.0％，以及余量的Ni。C 0.04% to 0.07%, Co 16.0% to 19.0%, Cr 8.0% to 12.0%, Mo 2.7% to 3.6%, W 3.4% to 5.0%, Ta 2.8% to 3.6%, Al 3.1% to 4.0%, Ti 3.0%～4.0%, Nb 1.6%～2.8%, Hf 0.2%～0.4%, Zr 0.01%～0.06%, B 0.01%～0.06%, Os 0.3%～3.0% and/or Ru0.5%～3.0 %, and the balance of Ni.
本发明的主要技术方案是通过控制Cr、Mo、W、Ru含量以降低拓扑密排(TCP)相析出倾向，同时通过添加固溶强化元素(Co、Cr、Mo、W、Ru)、γ′相形成元素(Al、Ti、Nb、Ta、Hf)和晶界强化元素(Zr、B)来实现合金的高的高温抗拉强度和屈服强度，以及优异的高温持久强度，从而获得具有良好的综合性能的成分范围。由于粉末高温合金的微米级预合金粉末在高冷速下冷却形成，使得合金成分均匀，微观组织均匀，析出相呈弥散分布，消除了宏观偏析，改善热加工性能，可以进一步提高合金化程度，使合金具有良好的拉伸心梗、高温持久性能和抗蠕变性能。通过协调控制Co、Cr、Mo、W、Ta等元素含量，降低TCP相析出倾向，改善合金的高温组织稳定性。The main technical scheme of the present invention is to reduce the precipitation tendency of topologically densely packed (TCP) phase by controlling the contents of Cr, Mo, W and Ru, and at the same time, by adding solid solution strengthening elements (Co, Cr, Mo, W, Ru), γ′ Phase forming elements (Al, Ti, Nb, Ta, Hf) and grain boundary strengthening elements (Zr, B) to achieve high high temperature tensile strength and yield strength of the alloy, as well as excellent high temperature endurance Composition range for comprehensive properties. Because the micron-scale pre-alloyed powder of the powder superalloy is formed by cooling at a high cooling rate, the alloy composition is uniform, the microstructure is uniform, and the precipitation phase is dispersed, which eliminates the macrosegregation, improves the hot working performance, and can further improve the alloying degree. The alloy has good tensile myocardial infarction, high temperature durability and creep resistance. By coordinating and controlling the content of Co, Cr, Mo, W, Ta and other elements, the tendency of TCP phase precipitation is reduced and the high temperature microstructure stability of the alloy is improved.
可选地，所述镍基粉末高温合金中Co、Cr、Mo、W的总质量分数为30％～38％。Optionally, the total mass fraction of Co, Cr, Mo, and W in the nickel-based powder superalloy is 30% to 38%.
可选地，所述镍基粉末高温合金中Co、Cr、Mo、W的总质量分数为32％～36％。Optionally, the total mass fraction of Co, Cr, Mo, and W in the nickel-based powder superalloy is 32% to 36%.
可选地，所述镍基粉末高温合金中W、Ta、Ru的总质量分数为8.5％～14.0％。Optionally, the total mass fraction of W, Ta and Ru in the nickel-based powder superalloy is 8.5% to 14.0%.
可选地，所述镍基粉末高温合金中W、Ta、Ru的总质量分数为9.0％～12.0％。Optionally, the total mass fraction of W, Ta and Ru in the nickel-based powder superalloy is 9.0% to 12.0%.
可选地，所述镍基粉末高温合金的主要析出相包括γ基体、γ′相、MC以及M3B2相。Optionally, the main precipitation phases of the nickel-based powder superalloy include γ matrix, γ' phase, MC and M 3 B 2 phase.
本发明合金的显微组织主要由γ、γ′、MC和M3B2相组成，γ′相的组成为(Ni,Co)3(Al,Ti,Ta,Nb,Hf)型，MC型碳化物的组成为(Ti,Ta,Nb,Hf)C型。The microstructure of the alloy of the invention is mainly composed of γ, γ′, MC and M 3 B 2 phases, and the composition of γ′ phase is (Ni, Co) 3 (Al, Ti, Ta, Nb, Hf) type, MC type The composition of carbide is (Ti, Ta, Nb, Hf)C type.
可选地，按质量分数计，所述镍基粉末高温合金中γ′相含量为55％～65％，所述γ′相的完全溶解温度为1180℃～1220℃。Optionally, in terms of mass fraction, the content of the γ' phase in the nickel-based powder superalloy is 55% to 65%, and the complete dissolution temperature of the γ' phase is 1180°C to 1220°C.
可选地，所述镍基粉末高温合金中γ′相的含量为60％，所述γ′相的完全溶解温度为1200℃～1220℃。Optionally, the content of the γ' phase in the nickel-based powder superalloy is 60%, and the complete dissolution temperature of the γ' phase is 1200°C to 1220°C.
可选地，当所述镍基粉末高温合金中含有Ru时，所述镍基粉末高温合金的γ基体中Ru的质量分数为0.30％～1.65％；和/或Optionally, when the nickel-based powder superalloy contains Ru, the mass fraction of Ru in the γ matrix of the nickel-based powder superalloy is 0.30% to 1.65%; and/or
当所述镍基粉末高温合金中含有Os时，所述镍基粉末高温合金的γ基体中Os的质量分数为0.24％～2.1％。When the nickel-based powder superalloy contains Os, the mass fraction of Os in the γ matrix of the nickel-based powder superalloy is 0.24% to 2.1%.
Ru降低难熔元素在γ相中的过饱和度，并能抑制TCP相等有害相的析出，提高合金显微组织的稳定性。同时Ru作为一种有效的固溶强化元素对γ相和γ′相的强化均起到了很显著的作用，提高合金的抗蠕变性能和持久性能。因此，在粉末高温合金中添加合适含量的元素Ru，可以提高合金的组织稳定性，同时提高合金的高温力学性能。Ru reduces the supersaturation of refractory elements in the γ phase, and can inhibit the precipitation of harmful phases such as TCP, and improve the stability of the alloy microstructure. At the same time, Ru, as an effective solid solution strengthening element, plays a significant role in strengthening both the γ phase and the γ′ phase, and improves the creep resistance and durability of the alloy. Therefore, adding a suitable content of Ru in the powder superalloy can improve the microstructure stability of the alloy and improve the high temperature mechanical properties of the alloy at the same time.
Os和Ru同属于Ⅷ族元素，且与ⅦB族的Re元素相毗邻。Os元素的熔点和原子半径介于Re和Ru之间，晶体结构与Re和Ru相同，均为HCP结构。由此推断Os在镍基高温合金中的强化效果与Re、Ru类似。同时，由第一性原理计算可知，元素Os具有很高的强化效果。在合金铸态组织中，利用枝晶间与枝晶干的成分计算元素的偏析系数ks＝C枝晶间/C枝晶干，由结果可知，Os在枝晶间偏析(正偏析)，Os对Al、Ti、Nb、Ta、Hf的偏析影响较大，使Al由偏析于枝晶干转变为枝晶间，Ta则由偏析于枝晶间转变为枝晶干，加剧了Ti、Nb向枝晶间偏析，减弱了Hf向枝晶间偏析。Os and Ru both belong to group VIII elements and are adjacent to the Re element of group VIIB. The melting point and atomic radius of Os element are between Re and Ru, and the crystal structure is the same as that of Re and Ru, both of which are HCP structures. Therefore, it is inferred that the strengthening effect of Os in nickel-based superalloys is similar to that of Re and Ru. At the same time, it can be seen from the first-principles calculations that the element Os has a high strengthening effect. In the as-cast structure of the alloy, the segregation coefficient ks=C interdendritic/C dendrite is calculated by using the composition of interdendritic and dendrite trunk. It has a great influence on the segregation of Al, Ti, Nb, Ta, and Hf, so that Al changes from segregation in dendrites to interdendrites, and Ta changes from segregation in dendrites to dendrites, which intensifies the tendency of Ti and Nb. The interdendritic segregation weakens the Hf segregation into the interdendritic.
在合金热处理态组织中，Os主要存在于γ基体中，其次存在于γ′相中，Os不存在于MC型碳化物中；Os使γ基体中的Co、Cr、Mo和W元素比例有所增加，Nb元素有所减少，其余合金元素分配比例变化不大。由此可知，Os主要起固溶强化作用。In the heat-treated structure of the alloy, Os mainly exists in the γ matrix, followed by the γ' phase, and Os does not exist in the MC-type carbide; Os makes the proportion of Co, Cr, Mo and W in the γ matrix to some extent. With the increase, the Nb element has decreased, and the distribution ratio of the remaining alloy elements has little change. From this, it can be seen that Os mainly plays the role of solid solution strengthening.
可选地，所述镍基粉末高温合金的最高工作温度在815℃以上。Optionally, the maximum working temperature of the nickel-based powder superalloy is above 815°C.
根据本发明的另一目的，提供了上述任一镍基粉末高温合金的制备方法，所述方法包括步骤：According to another object of the present invention, a method for preparing any of the above nickel-based powder superalloys is provided, the method comprising the steps of:
a)按质量分数配比将各成分混合熔炼，并获得合金前驱料；a) mix and smelt the components according to the mass fraction ratio, and obtain the alloy precursor;
b)将步骤a)中获得的所述合金前驱料进行制粉、筛分、静电处理，获得合金粉末；b) subjecting the alloy precursor obtained in step a) to powder milling, sieving and electrostatic treatment to obtain alloy powder;
c)对步骤b)中获得的所述合金粉末进行真空脱气和封焊后，进行热等静压成形，获得锭坯；c) After vacuum degassing and sealing welding of the alloy powder obtained in step b), hot isostatic pressing is performed to obtain an ingot;
d)对步骤c)中获得的所述锭坯进行热处理，获得所述镍基粉末高温合金。d) heat-treating the ingot obtained in step c) to obtain the nickel-based powder superalloy.
可选地，在所述步骤a)中，所述合金前驱料采用真空感应熔炼工艺获得。Optionally, in the step a), the alloy precursor is obtained by a vacuum induction melting process.
可选地，在所述步骤b)中，所述制粉采用等离子旋转电极法进行；所述合金粉末的粒度为50μm～150μm。Optionally, in the step b), the powdering is performed by a plasma rotating electrode method; the particle size of the alloy powder is 50 μm˜150 μm.
可选地，在所述步骤c)中，所述热等静压成形的条件为：温度为1170℃～1230℃，压力为120MPa～140MPa，保温时间为2h～4h。Optionally, in the step c), the conditions of the hot isostatic pressing are as follows: the temperature is 1170°C-1230°C, the pressure is 120MPa-140MPa, and the holding time is 2h-4h.
可选地，在所述步骤d)中，所述热处理包括固溶热处理和时效热处理。Optionally, in the step d), the heat treatment includes solution heat treatment and aging heat treatment.
可选地，所述固溶热处理的条件为：1190℃～1230℃/2h～10h/空冷。Optionally, the conditions of the solution heat treatment are: 1190°C～1230°C/2h～10h/air cooling.
可选地，所述时效热处理包括多级时效热处理，优选为两级时效热处理；所述时效热处理的条件为：860℃～940℃/2h～6h/空冷+740℃～780℃/12h～22h/空冷。Optionally, the aging heat treatment includes multi-stage aging heat treatment, preferably two-stage aging heat treatment; the conditions of the aging heat treatment are: 860℃～940℃/2h～6h/air cooling+740℃～780℃/12h～22h / air cooling.
作为一种实施方式，镍基粉末高温合金的制备方法，所述方法包括步骤：As an embodiment, a method for preparing a nickel-based powder superalloy, the method includes the steps:
S1.按粉末高温合金的化学成分及其质量分数配制原料，采用真空感应熔炼工艺制备合金棒料；S1. Prepare raw materials according to the chemical composition and mass fraction of powder superalloy, and prepare alloy bars by vacuum induction melting process;
S2.将合金棒料采用等离子旋转电极法制备高温合金粉末，合金粉末经过筛分、静电处理，得到粒度为50～150μm的成品粉末；S2. The alloy bar material is prepared by the plasma rotating electrode method to prepare the superalloy powder, and the alloy powder is sieved and electrostatically treated to obtain a finished powder with a particle size of 50-150 μm;
S3.合金粉末装入低碳钢包套，进行真空脱气和封焊；S3. The alloy powder is loaded into the low carbon steel ladle, and vacuum degassing and sealing welding are carried out;
S4.对封焊后的合金粉末进行热等静压成形，得到锭坯；具体地，热等静压条件为：1170℃～1230℃，压力120MPa～140MPa，保温时间2h～4h；S4. Hot isostatic pressing is performed on the alloy powder after sealing and welding to obtain an ingot; specifically, the hot isostatic pressing conditions are: 1170 ℃～1230 ℃, pressure 120MPa～140MPa, holding time 2h～4h;
S5.对成形后的锭坯进行热处理，得到粉末高温合金制件。热处理包括固溶热处理和时效热处理；具体地，固溶热处理条件为：1190℃～1230℃/2h～10h/空冷，时效热处理包括两级时效热处理，时效热处理制度为：860℃～940℃/2h～6h/空冷+740℃～780℃/12h～22h/空冷。S5. Perform heat treatment on the formed ingot to obtain a powdered superalloy product. The heat treatment includes solution heat treatment and aging heat treatment; specifically, the solution heat treatment conditions are: 1190℃～1230℃/2h～10h/air cooling, the aging heat treatment includes two-stage aging heat treatment, and the aging heat treatment system is: 860℃～940℃/2h ~6h/air cooling+740℃～780℃/12h～22h/air cooling.
根据本发明的又一目的，提供了应用上述任一镍基粉末高温合金的航空设备。According to another object of the present invention, there is provided aviation equipment using any of the above nickel-based powder superalloys.
可选地，所述航空设备为航空发动机。Optionally, the aeronautical equipment is an aeroengine.
可选地，所述航空设备为航空发动机涡轮盘。Optionally, the aviation equipment is an aero-engine turbine disk.
与现有技术相比，本发明的有益效果为：Compared with the prior art, the beneficial effects of the present invention are:
(1)本发明提供的镍基粉末高温合金具有优异综合性能的成分构成及含量，这赋予了所述镍基粉末高温合金优异的高温抗拉强度、屈服强度和高温持久性能以及更高的最高工作温度。(1) The nickel-based powder superalloy provided by the present invention has the composition and content of components with excellent comprehensive properties, which endow the nickel-based powder superalloy with excellent high-temperature tensile strength, yield strength and high-temperature durability, as well as higher maximum Operating temperature.
(2)本发明提供的镍基粉末高温合金通过控制Cr、Mo、W、Ru含量以降低拓扑密排(TCP)相析出倾向，同时通过添加固溶强化元素(Co、Cr、Mo、W、Ru)、γ′相形成元素(Al、Ti、Nb、Ta、Hf)和晶界强化元素(Zr、B)来实现合金的高的高温抗拉强度和屈服强度，以及优异的高温持久强度，通过协调控制Co、Cr、Mo、W、Ta等元素含量，降低TCP相析出倾向，改善合金的高温组织稳定性。(2) The nickel-based powder superalloy provided by the present invention reduces the precipitation tendency of topologically close packed (TCP) phase by controlling the contents of Cr, Mo, W and Ru, and at the same time, by adding solid solution strengthening elements (Co, Cr, Mo, W, Ru), γ' phase forming elements (Al, Ti, Nb, Ta, Hf) and grain boundary strengthening elements (Zr, B) to achieve high high temperature tensile strength and yield strength of the alloy, as well as excellent high temperature endurance strength, By coordinating and controlling the content of Co, Cr, Mo, W, Ta and other elements, the tendency of TCP phase precipitation is reduced and the high temperature microstructure stability of the alloy is improved.
(3)本发明提供的镍基粉末高温合金的最高工作温度可以达到815℃以上，能够满足航空发动机的对高温下材料性能的苛刻要求，可以用作815℃以上的温度场景下的航空高温材料。(3) The maximum working temperature of the nickel-based powder superalloy provided by the present invention can reach above 815°C, which can meet the strict requirements of aero-engines for material properties at high temperatures, and can be used as aeronautical high-temperature materials in temperature scenarios above 815°C .
(4)本发明提供的镍基粉末高温合金的制备方法高效易行、重现性好，制备得到的镍基粉末高温合金显微组织结构稳定性高。(4) The preparation method of the nickel-based powder superalloy provided by the present invention is efficient, easy to implement, and has good reproducibility, and the prepared nickel-based powder superalloy has high microstructure stability.
附图说明Description of drawings
为了更清楚地说明本发明具体实施方式或现有技术中的技术方案，下面将对具体实施方式或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图是本发明的一些实施方式，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。In order to illustrate the specific embodiments of the present invention or the technical solutions in the prior art more clearly, the following briefly introduces the accompanying drawings that need to be used in the description of the specific embodiments or the prior art. Obviously, the accompanying drawings in the following description The drawings are some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings without creative efforts.
图1为本发明一种实施方式中镍基粉末高温合金的热处理态的金相组织结构表征结果；Fig. 1 is the metallographic structure characterization result of the heat treatment state of nickel-based powder superalloy in one embodiment of the present invention;
图2为本发明一种实施方式中镍基粉末高温合金经815℃/3000h时效热处理后的金相组织结构表征结果；Fig. 2 is the metallographic structure characterization result of the nickel-based powder superalloy after aging heat treatment at 815°C/3000h in an embodiment of the present invention;
图3为本发明一种实施方式中镍基粉末高温合金经850℃/500h时效热处理后的金相组织结构表征结果。FIG. 3 is the metallographic structure characterization result of the nickel-based powder superalloy after aging heat treatment at 850°C/500h in one embodiment of the present invention.
具体实施方式Detailed ways
下面将结合实施例对本发明的实施方案进行详细描述，但是本领域技术人员将会理解，下列实施例仅用于说明本发明，而不应视为限制本发明的范围。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市购获得的常规产品。The embodiments of the present invention will be described in detail below with reference to the examples, but those skilled in the art will understand that the following examples are only used to illustrate the present invention and should not be regarded as limiting the scope of the present invention. If the specific conditions are not indicated in the examples, it is carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used without the manufacturer's indication are conventional products that can be obtained from the market.
实施例1镍基粉末高温合金的制备Example 1 Preparation of nickel-based powder superalloy
以表1中所列的成分及其含量为原料制备1#～5#镍基粉末高温合金。Using the components and their contents listed in Table 1 as raw materials, 1 # to 5 # nickel-based powder superalloys were prepared.
表1镍基粉末高温合金样品的成分及制备条件Table 1 Composition and preparation conditions of nickel-based powder superalloy samples
制备方法具体如下：The preparation method is as follows:
S1.按粉末高温合金的化学成分及其质量分数配制原料，采用25kg真空感应熔炼工艺制备合金棒料；S1. Prepare raw materials according to the chemical composition and mass fraction of powder superalloy, and prepare alloy bars by 25kg vacuum induction melting process;
S2.将合金棒料采用等离子旋转电极法制备高温合金粉末，合金粉末经过筛分、静电处理，得到粒度为50μm～150μm的成品粉末；S2. The alloy bar is prepared by the plasma rotating electrode method to prepare the superalloy powder, and the alloy powder is sieved and electrostatically treated to obtain a finished powder with a particle size of 50 μm to 150 μm;
S3.合金粉末装入低碳钢包套，进行真空脱气和封焊；S3. The alloy powder is loaded into the low carbon steel ladle, and vacuum degassing and sealing welding are carried out;
S4.对封焊后的合金粉末进行热等静压成形，得到锭坯；S4. Perform hot isostatic pressing on the alloy powder after sealing and welding to obtain an ingot;
S5.对成形后的锭坯进行热处理，得到粉末高温合金制件；热处理包括固溶热处理和时效热处理。S5. Perform heat treatment on the formed ingot to obtain a powder superalloy product; the heat treatment includes solution heat treatment and aging heat treatment.
实验例1镍基粉末高温合金的金相结构表征Experimental Example 1 Metallographic structure characterization of nickel-based powder superalloys
采用Olympus GM-7型金相显微镜观察热处理态和长期时效后合金的显微组织，表征实施例1中制备得到的1#～5#镍基粉末高温合金的金相结构。An Olympus GM-7 metallographic microscope was used to observe the microstructure of the alloy in the heat-treated state and after long-term aging, and to characterize the metallographic structure of the 1 # to 5 # nickel-based powder superalloy prepared in Example 1.
以4#镍基粉末高温合金为典型，其热处理态的金相结构如图1所示；4#镍基粉末高温合金经815℃/3000h时效后以及经850℃/500h时效后的金相结构分别如图2和图3所示。Taking 4 # nickel-based powder superalloy as a typical example, the metallographic structure of its heat treatment state is shown in Figure 1; the metallographic structure of 4 # nickel-based powder superalloy after aging at 815℃/3000h and after aging at 850℃/500h As shown in Figure 2 and Figure 3, respectively.
本发明提供的镍基粉末高温合金的显微组织主要由γ、γ′、MC和M3B2相组成，γ′相的组成为(Ni,Co)3(Al,Ti,Ta,Nb,Hf)型，MC型碳化物的组成为(Ti,Ta,Nb,Hf)C型。The microstructure of the nickel-based powder superalloy provided by the invention is mainly composed of γ, γ′, MC and M3B2 phases, and the composition of the γ′ phase is (Ni, Co) 3 (Al, Ti, Ta, Nb, Hf) type , the composition of MC-type carbide is (Ti, Ta, Nb, Hf) C type.
1#镍基粉末高温合金的γ′相含量为60％(质量分数)，γ′相完全溶解温度为1200～1220℃，约有80％的Os进入γ基体，即γ基体中Os的质量分数为0.32％。1 # Nickel-based powder superalloy has a γ' phase content of 60% (mass fraction), a complete dissolution temperature of the γ' phase at 1200-1220 °C, and about 80% of the Os enters the γ matrix, that is, the mass fraction of Os in the γ matrix. is 0.32%.
2#镍基粉末高温合金的γ′相含量为60％(质量分数)，γ′相完全溶解温度为1200～1220℃，约有78％的Os进入γ基体，即γ基体中Os的质量分数为1.4％。2 # The content of γ' phase in nickel-based powder superalloy is 60% (mass fraction), the complete dissolution temperature of γ' phase is 1200-1220 ℃, and about 78% of Os enters the γ matrix, that is, the mass fraction of Os in the γ matrix was 1.4%.
3#镍基粉末高温合金的γ′相含量为60％(质量分数)，γ′相完全溶解温度为1180～1200℃，约有58％的Ru进入γ基体，即γ基体中Ru的质量分数为0.35％。3 # Nickel-based powder superalloy has a γ' phase content of 60% (mass fraction), the complete dissolution temperature of γ' phase is 1180-1200 ℃, and about 58% of Ru enters the γ matrix, that is, the mass fraction of Ru in the γ matrix is 0.35%.
4#镍基粉末高温合金的γ′相含量为60％(质量分数)，γ′相完全溶解温度为1180～1200℃，约有55％的Ru进入γ基体，即γ基体中Ru的质量分数为1.24％。The γ' phase content of 4 # nickel-based powder superalloy is 60% (mass fraction), the complete dissolution temperature of γ' phase is 1180-1200 ℃, and about 55% of Ru enters the γ matrix, that is, the mass fraction of Ru in the γ matrix was 1.24%.
由图2和图3可知，镍基粉末高温合金经815℃/3000h、850℃/500h时效热处理后无TCP相析出，可见其在815℃下具有优异的高温组织稳定性。It can be seen from Figure 2 and Figure 3 that the nickel-based powder superalloy has no TCP phase precipitation after aging heat treatment at 815°C/3000h and 850°C/500h, which shows that it has excellent high temperature microstructure stability at 815°C.
实验例2镍基粉末高温合金的性能表征Experimental example 2 Performance characterization of nickel-based powder superalloys
采用NCS GNT100电子拉伸试验机、GNCJ-30机械式高温持久蠕变试验机测试实施例1中制备得到的1#～5#镍基粉末高温合金的力学性能。The mechanical properties of the 1 # to 5 # nickel-based powder superalloys prepared in Example 1 were tested by NCS GNT100 electronic tensile testing machine and GNCJ-30 mechanical high temperature durable creep testing machine.
其中，1#～5#镍基粉末高温合金的室温拉伸性能、760℃拉伸性能、815℃拉伸性能、815℃/450MPa持久性能分别列于表2、表3、表4、表5中。Among them, the room temperature tensile properties, 760 °C tensile properties, 815 °C tensile properties, and 815 °C/450MPa durability properties of 1 # ~ 5 # nickel-based powder superalloys are listed in Table 2, Table 3, Table 4, Table 5, respectively middle.
表2镍基粉末高温合金的室温拉伸性能Table 2 Room temperature tensile properties of nickel-based powder superalloys
表3镍基粉末高温合金的760℃拉伸性能Table 3 Tensile properties of nickel-based powder superalloys at 760℃
表4镍基粉末高温合金的815℃拉伸性能Table 4 Tensile properties of nickel-based powder superalloys at 815℃
表5镍基粉末高温合金的815℃/450MPa持久性能Table 5 815℃/450MPa durability performance of nickel-based powder superalloys
现有的粉末高温合金ME501[A.Powell,K.Bain,A.Wessman,et al.Advancedsupersolvus nickel powder disk alloy DOE:chemistry,properties,phaseformations and thermal stability[C].Superalloys 2016:189-197；D.P.Mourer,K.R.Bain.Nickel-based alloy,processing therefor and components formedthereof:US 8613810[P].2013-12-24]，其760℃的抗拉强度、屈服强度分别为1186MPa和1041MPa，815℃的抗拉强度、屈服强度分别为993MPa和903MPa，815℃/345MPa的持久寿命为532h。Existing powder superalloy ME501[A.Powell,K.Bain,A.Wessman,et al.Advancedsupersolvus nickel powder disk alloy DOE:chemistry,properties,phaseformations and thermal stability[C].Superalloys 2016:189-197;D.P. Mourer, K.R.Bain.Nickel-based alloy, processing therefor and components formed thereof: US 8613810[P].2013-12-24], its tensile strength and yield strength at 760℃ are 1186MPa and 1041MPa respectively, and the tensile strength at 815℃ The strength and yield strength are 993MPa and 903MPa respectively, and the durable life at 815℃/345MPa is 532h.
由表3和表4中数据可知，与现有的粉末高温合金ME501相比，本发明提供的镍基粉末高温合金在760℃、810℃的抗拉强度、屈服强度有较大幅度提高；由表5中数据可知，本发明提供的1#、2#镍基粉末高温合金在815℃的持久强度是ME501合金的1.35倍以上，3#、4#、5#镍基粉末高温合金在815℃的持久强度是ME501合金的1.29倍以上。可见，本发明提供的镍基粉末高温合金具有优异的力学性能。It can be seen from the data in Tables 3 and 4 that compared with the existing powder superalloy ME501, the nickel-based powder superalloy provided by the present invention has a relatively large increase in tensile strength and yield strength at 760° C. and 810° C.; It can be seen from the data in Table 5 that the lasting strength of the 1 # and 2 # nickel-based powder superalloys provided by the present invention at 815°C is more than 1.35 times that of the ME501 alloy, and the 3 # , 4 # and 5 # nickel-based powder superalloys are at 815° C. The lasting strength is more than 1.29 times that of ME501 alloy. It can be seen that the nickel-based powder superalloy provided by the present invention has excellent mechanical properties.
最后应说明的是：以上各实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述各实施例对本发明进行了详细的说明，但本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分或者全部技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand: It is still possible to modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements to some or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the technical solutions of the embodiments of the present invention. range.
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