含铼镍基单晶高温合金组织稳定性及低铼成分的热力学设计
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摘要
为了进一步提高镍基单晶高温合金的承温能力,满足于航空发动机对于提高涡轮入口温度的需要,通常在镍基单晶高温合金中加入难熔元素Re、W、Ta、Mo等,以提高γ基体相的固溶强化作用和γ'相析出强化作用,尤其是Re元素的加入,大大提高了合金的高温强度。但这些难熔元素的加入在提高材料承温能力的同时促进了合金在高温服役时TCP相的生成,影响了γ/γ'相的微观结构稳定性,同时对合金的制备和加工亦带来了不利的影响。此外,由于Re不仅价格昂贵而且密度较大,Re元素的添加大大提高了合金的成本和密度,这势必限制了其在合金中的大量使用。因此,本文通过实验研究和热力学计算结合的方法,研究了一种含铼镍基单晶高温合金的组织稳定性以及合金元素在γ/γ'两相及界面处的分布规律;并且尝试了将合金中的Re含量降低到1wt.%,而微调其他合金元素的相对含量,以取代Re元素,设计了几种低铼含量且承温能力达到二代水平的单晶高温合金。
用光加热悬浮区熔法制备了一种铼含量为5wt.%的镍基单晶高温合金。借助扫描电镜(SEM)、透射电镜(TEM)、扫描透射电镜(STEM)以及能谱仪(EDS),研究了不同热处理条件下,该合金的微观组织演化规律以及合金元素在γ/γ'两相及界面处的分布规律。在该合金中观察到了相分离现象(即γ'相中析出γ相),且对相分离的过程、产生原因以及其对微观组织演化的影响进行了分析。实验结果表明:一次时效后,γ'相主要以立方形形态析出,且无相分离现象出现,合金元素Re、Co、Cr、Mo富集于γ基体相,而合金元素Ni、Al富集于γ'析出相,此外,W元素平均分配于γ/γ'两相中。二次时效后,有细小的近球形γ'相二次析出,且出现了相分离现象,合金元素Re、Co、Cr、Mo富集于γ基体相,而合金元素Ni和Al富集于γ'析出相,此外,W元素富集在γ/γ'界面附近处,且其在γ'析出相中的含量高于其在γ基体相中的含量。
另外,本文利用热力学软件JMatPro和相应的镍基高温合金数据库分析总结了几代典型镍基单晶高温合金与性能相关的参数,如合金初熔温度、密度、γ'相体积分数、γ/γ'相错配度、TCP相含量、热加工窗口以及糊状区区间等,且从单晶叶片设计要求、微观组织稳定性要求和加工工艺性能要求三方面出发,制定了合金设计相应的热力学判据。并在此基础上,通过固定Re、Al、Cr等部分合金元素含量,调整W、Mo、Co、Ta等合金元素的相对含量,在二代单晶合金的基础上降低铼元素含量至1wt.%,尝试设计了一系列不同成分的合金,且利用JMatPro对合金初熔温度、密度、γ'相体积分数、γ/γ'错配度、TCP相含量、热加工窗口以及糊状区区间等进行了分析,得到了几组低铼且承温能力达到二代单晶水平的合金成分。
In order to improve the temperature capability of nickel-based single crystal superalloys to meet the need for an increased turbine entry temperature, refractory elements such as Re, W, Ta, Mo, most notably Re, are added to enhance the high-temperature properties through both the solid solution strengthing in theγmatrix and precipitation strengthening via theγ' formation. The additions of these refractory elements improve the temperature capability of materials, and in the meanwhile increase the tendency of forming topologically close-packed (TCP) phases during prolonged exposures to elevated temperatures in service. This results in destabilization of theγ/γ' microstructure and gives rise to the negative effect on the preparation and processing of the alloys. Besides, Re additions increase the cost and density of the alloys since Re is both expensive and heavy. These drawbacks limit Re addition in the nickel-based single crystal superalloys. In this paper, a Re-containing nickel-based single crystal superalloy has been studied based on thermodynamic calculation and experiments. The microstructure stability ofγ/γ' phase and elemental partitioning both betweenγandγ' phase and at its interface have been investigated. In addition, attempts have been made to the design of some low Re-containing nickel-based single crystal superalloys which bear a temperature capability of the second-generation nickel-based single crystal superalloys. The Re content in the alloys was set to 1 wt.%, and the contents of other alloying elements were slightly modified to compensate for the strengthening effect from Re.
A nickel-based single crystal superalloy containing 5 wt.% Re has been prepared by optical heating floating zone method. Theγ/γ' microstructure and the elemental distribution in the microstructure have been investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectrometry (EDS) using specimens under different heat treatment conditions. In the studied alloy, phase-separation (γphases precipitate withinγ' precipitates) was observed, and its process, mechanism and the effects on the microstructural evolution have been systematically investigated. After the first-step aging at 1100γC,γ' phases were found to mainly precipitate in cuboidal shape and no phase-separation was observed. Re, Co, Cr and Mo were enriched in theγmatrix, while Ni and Al were concentrated in theγ' phase. W partitioned equally to theγandγ' phase. After second-step aging at 870γC, fineγ' phases were further precipitated in spherical shape and phase-separation withinγ' precipitates was observed. The elements of Re, Co, Cr, Mo, were enriched in theγmatrix, while Ni and Al were concentrated in theγ' phase. Besides, there was certain enrichment of W in the vicinity of theγ/γ' interface, and the contents of W in theγ' phase was higher than that in theγmatrix.
Besides, some typical nickel-based single crystal superalloys have been studied by thermodynamic calculation, including the incipient melting temperature, density, the volume fraction ofγ', theγ/γ' misfit, the TCP contents, heat treatment window, and the temperature range of mush zone etc. All the thermodynamic properties have been investigated using JMatPro and the latest relevant database for nickel-based superalloys. According to requests for single-crystal blade design,γ/γ' microstructure stability and process-ability, design criteria of the alloys were made. Based on these, a series of alloys with different contents were designed by fixing the contents of some elements such as Re, Al, Cr, etc. and changing the relative contents of W, Mo, Co, Ta. The Re content was set to 1 wt.%. Meanwhile, the incipient melting temperature, density, the volume fraction ofγ', theγ/γ' misfit, TCP contents, heat treatment window, and the temperature range of mush zone of all the designed alloys were estimated by JMatPro. Finally, some low Re-containing alloys with reaching the temperature capability of second-generation nickel-based single crystal superalloys have been obtained.
用光加热悬浮区熔法制备了一种铼含量为5wt.%的镍基单晶高温合金。借助扫描电镜(SEM)、透射电镜(TEM)、扫描透射电镜(STEM)以及能谱仪(EDS),研究了不同热处理条件下,该合金的微观组织演化规律以及合金元素在γ/γ'两相及界面处的分布规律。在该合金中观察到了相分离现象(即γ'相中析出γ相),且对相分离的过程、产生原因以及其对微观组织演化的影响进行了分析。实验结果表明:一次时效后,γ'相主要以立方形形态析出,且无相分离现象出现,合金元素Re、Co、Cr、Mo富集于γ基体相,而合金元素Ni、Al富集于γ'析出相,此外,W元素平均分配于γ/γ'两相中。二次时效后,有细小的近球形γ'相二次析出,且出现了相分离现象,合金元素Re、Co、Cr、Mo富集于γ基体相,而合金元素Ni和Al富集于γ'析出相,此外,W元素富集在γ/γ'界面附近处,且其在γ'析出相中的含量高于其在γ基体相中的含量。
另外,本文利用热力学软件JMatPro和相应的镍基高温合金数据库分析总结了几代典型镍基单晶高温合金与性能相关的参数,如合金初熔温度、密度、γ'相体积分数、γ/γ'相错配度、TCP相含量、热加工窗口以及糊状区区间等,且从单晶叶片设计要求、微观组织稳定性要求和加工工艺性能要求三方面出发,制定了合金设计相应的热力学判据。并在此基础上,通过固定Re、Al、Cr等部分合金元素含量,调整W、Mo、Co、Ta等合金元素的相对含量,在二代单晶合金的基础上降低铼元素含量至1wt.%,尝试设计了一系列不同成分的合金,且利用JMatPro对合金初熔温度、密度、γ'相体积分数、γ/γ'错配度、TCP相含量、热加工窗口以及糊状区区间等进行了分析,得到了几组低铼且承温能力达到二代单晶水平的合金成分。
In order to improve the temperature capability of nickel-based single crystal superalloys to meet the need for an increased turbine entry temperature, refractory elements such as Re, W, Ta, Mo, most notably Re, are added to enhance the high-temperature properties through both the solid solution strengthing in theγmatrix and precipitation strengthening via theγ' formation. The additions of these refractory elements improve the temperature capability of materials, and in the meanwhile increase the tendency of forming topologically close-packed (TCP) phases during prolonged exposures to elevated temperatures in service. This results in destabilization of theγ/γ' microstructure and gives rise to the negative effect on the preparation and processing of the alloys. Besides, Re additions increase the cost and density of the alloys since Re is both expensive and heavy. These drawbacks limit Re addition in the nickel-based single crystal superalloys. In this paper, a Re-containing nickel-based single crystal superalloy has been studied based on thermodynamic calculation and experiments. The microstructure stability ofγ/γ' phase and elemental partitioning both betweenγandγ' phase and at its interface have been investigated. In addition, attempts have been made to the design of some low Re-containing nickel-based single crystal superalloys which bear a temperature capability of the second-generation nickel-based single crystal superalloys. The Re content in the alloys was set to 1 wt.%, and the contents of other alloying elements were slightly modified to compensate for the strengthening effect from Re.
A nickel-based single crystal superalloy containing 5 wt.% Re has been prepared by optical heating floating zone method. Theγ/γ' microstructure and the elemental distribution in the microstructure have been investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectrometry (EDS) using specimens under different heat treatment conditions. In the studied alloy, phase-separation (γphases precipitate withinγ' precipitates) was observed, and its process, mechanism and the effects on the microstructural evolution have been systematically investigated. After the first-step aging at 1100γC,γ' phases were found to mainly precipitate in cuboidal shape and no phase-separation was observed. Re, Co, Cr and Mo were enriched in theγmatrix, while Ni and Al were concentrated in theγ' phase. W partitioned equally to theγandγ' phase. After second-step aging at 870γC, fineγ' phases were further precipitated in spherical shape and phase-separation withinγ' precipitates was observed. The elements of Re, Co, Cr, Mo, were enriched in theγmatrix, while Ni and Al were concentrated in theγ' phase. Besides, there was certain enrichment of W in the vicinity of theγ/γ' interface, and the contents of W in theγ' phase was higher than that in theγmatrix.
Besides, some typical nickel-based single crystal superalloys have been studied by thermodynamic calculation, including the incipient melting temperature, density, the volume fraction ofγ', theγ/γ' misfit, the TCP contents, heat treatment window, and the temperature range of mush zone etc. All the thermodynamic properties have been investigated using JMatPro and the latest relevant database for nickel-based superalloys. According to requests for single-crystal blade design,γ/γ' microstructure stability and process-ability, design criteria of the alloys were made. Based on these, a series of alloys with different contents were designed by fixing the contents of some elements such as Re, Al, Cr, etc. and changing the relative contents of W, Mo, Co, Ta. The Re content was set to 1 wt.%. Meanwhile, the incipient melting temperature, density, the volume fraction ofγ', theγ/γ' misfit, TCP contents, heat treatment window, and the temperature range of mush zone of all the designed alloys were estimated by JMatPro. Finally, some low Re-containing alloys with reaching the temperature capability of second-generation nickel-based single crystal superalloys have been obtained.
引文
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