Intermetallic 120 (2020) 106748 Contents lists available at ScienceDirect, Intermetallics journal homepage: hp:/iwww.elsevier-com/locatelintermet t A multi-phase CrMnFeCoNiAlos high-entropy alloy with high strength at intermediate temperature Lijing Lin, Xin Xian", Zhihong Zhong """, Chang Chen”, Zhixiong Zhu", Yucheng Wu", Peter K. Liaw“ 1 Seka! of Mati Sec and ageing, Heel Une of Taig fe, 29000, na > nga Rear Cer of ig eramance Copper Ally Matron Pring Myo uation, Heft Unie of Tcl He, 29008, China « 2g J Toc Meat Ca,L Ha 319012, Can \Deprmanof Mani Sees ond Ege, Une of Terns Kasei TN, 97996, USA Tower gweneropy alloys iWighenropy alays with « superalloy Ike ierntuctare show excellent wchaical properties at clevted temperatures n this paper, a multi-phase high-ntropy alloy CrMnFeCONiAlag was developed, Based om the imroscructure characterization by XRD, SEM, Te and 3D-APT, it was found tat the alloy was composed of FCG phase, BOC phase, and B2 phase. The mechanical propertis evaluation showed thatthe alloy had high ‘compression yield strength of 1194 MPa at room temperature and could preserve high yield strength of 1070 ‘MPa nt 500°C. Further increase in the temperate Beyond 600°C resulted in alloy sotening. The aloy showed limited strain of 2.729 at room temperature, butt exhibited adequate deformability at elevated temperatures up 9 500 C (stain >20%). The strengthening mechanisms of the alloy at diferent tamperatures were dscsse, 1. Introduetion Inthe last decade, with the development of material-design concept, high-entropy alloys (HEAS) [5] have attracted considerable attention. [HIFAS vith high mixing entropies contained at least five principal ce ments and showed promising properties for a wide range of applications. For cxample, the combination of excellent thermal stability, high-temperature strength, and ductility of HEAS makes the alloys good ‘candidates for high-temperature applications (6,71. According to the previous studies [3-12], phase-structure types are the dominant factor in determining whe mechanical properties, It is known that the face-centered-cubic (FCC) structure has slip planes with the closest packing, while the body-centered-cubic (BCC) structire has no ‘lose-packed sip planes. The critical stress for slip inthe FCC sevetuce basically smaller than that inthe BCC structure. Thus, HEAs with a BCC structure usually exhibit high yield stength and limited ductiligy (1, while the FOCstructured HEAs have relatively low yield strength and high ductility (1. Hence, an alloy consisting of BCC and FCC phases is ‘expected to possess high strength and good ductility [15,]6]. As re ported by Tang ctl. (17), the compression yield strength of a FCC phase structured alloy Al sCOCrCuFeNi was low, but the ductility ofthe alloy was good. On the other hand, a dual-phase PCC 4 BCC structured AlCaCrCuFeNi alloy showed high compression yield strength at 600 °C (600 MPa), which was even higher than the yield strength of refractory Bigh-entropy alloy NbMoTaW atthe same temperature [1s]. Hence, the FCC ~ BOC dual-phase stractured HEAs may posses high strength and. 200d ductility, ithe volume faction ratio of FCC to BCC was proper. ‘Some efforts have been made to achieve the dual-phase structured HAs. Recently, the Als ;CoCHFesN\ alloy with a superaloy-like micro structure had been developed (19]. It was found that the cuboidal B2 (ordered BCC) precipitate coherently embedded in the BCC matrix, which was very similar to the microstructure of conventional Nicbase superalloys. During the deformation process, the dislocations mainly ‘moved inthe BCC channel, and the B2 precipitate effectively impede the ‘motion of dislocation, Hence the alloy showed both high strength and good ductility at elevated temperatures. By changing the alloy compo- Sitio, i is also possible to obtain eutectic HEAS with # dual-phase structure (20-22]. It was found that AICOCSFeNip alloy possessed a fine lamellar FCC/B2 microstructure. Eutectic HEAS showed an un- precedented combination of high tensile ductility and fracture strength atroom temperature, duc to the formation ofa mixed microstructure of alternating sof FCC and hard BCC phases [21,221 * Conespondlng author. School of Materials Sclence and Engineering, Hefel University of Techaolgy, Hefe! 230008, China mal dares short wo (2 Pong. Itps://doL.og/10.1016/.termet.2020.106744 Availabe online 17 February 2020, (0966-97956 2020 Heever Ld, Al rights reserve,In this poper, a superalloy-Lke microstructure of CrMnFeCoNiAlo7s alloy was proposed to acquire high strength at both room and inter mediate temperatures, The microstructure and mechanical properties were investigated by Xray difraction, scanning electron microscope, ‘three-dimensional stom probe tomography, transmission electron mi. ‘roscope and compression tests at different temperatures. The strengthening mechanisms ofthe alloy at different temperatures were also discussed. 2. Experimental The CrMaFeCoNiAly 5 ingot was prepared by arc-melting of high purity elements (+99.5 3). The button ingot was remelted five times to ensure the chemical homogeneity. The exystal structure of as-cast alloy was analyzed by X-ray diffraction (XRD) with a speed of 0.2°/ min. A Signa-Zess type scanning electron microscope (SEM) was used for the microstructural analysis. The element distribution and micro ‘composition were analyzed by the three-dimensional atom probe to rmography (3D-APT) (CAMECA LEAP4OOOHR) and energy dispersive spectrometry (EDS), The microstructure, phase structure, and disloc on distribution were also studied by the transmission electron micro scope (TEM) (FEI TECNAL G2 S-TWIN F20) and high resolution transmission eletron microscope (HR-TEM). The samples for the TEM ‘observation were fabricated by ion milling. The diameter and height of samples for compression tests was 3 mm and 6 mm, respectively. The ‘experiment was performed in a universal testing machine (SHIMADZU, ‘AG-X Plus 100 KN) wit a strain rate of 10°? 5, in the temperature range from room temperature to 900 °C. The fracture morphology was ‘examined by SEM. The 0.2% proof stress was measured a the yield strength. 3. Results and discussion 3.1, Crystal suture and mierosruture ig: | shows the XRD pattern of CrMnFeCoNiAlays alloy. For com parison, the XRD pattern of as-cast CrMnFeCoN alloy was as shown in ig. 1. The C2MnFeCoN alloy was confirmed to be the single-phase FCC structured alloy. For the GeMineCoNiAlo 75 alloy, besides the diffraction peaks corresponding to FCC phase, some peaks appeared at around 445° and around 82. These peaks were identified to be the peaks of [BCC phase, revealing that the alloy has a mixed structure of PCC and [BCC phases. The lattice parameter of FCC and BCC phase was caleulated Fee 2 @ |crimnFeConial,,, 2 mn ” em eH SitnFeConi 30 40 «80 GD 70 «BOD 100 28 (degree) pattern of CoinPeCoNt was also given for compare, rete 1202020) 106744 from the XRD patter to be 0.3621 + 0.003 nm and 0.2880 + 0,002 nm, respectively, which was similar to the results reported by other studies baa ‘hg, UG) isthe back-scattered electron SEM image of CrMneCo- NiAlg7s alloy. I¢ could be seen that the alloy consisted of light-gray (stripshaped) and gray phases. The SEM-EDS indicated that the light- gray phase contained high amounts of Fe, Cr, Mn and Co, while the ray phase was rch in Ni, Al, Cr and Fe, Ao eutecticlike structure was observe inside the gray regions. For more detail about the eutectic-ike strueture, TEM experiment was carried out and the bright field TEM. Cr ern oe Td Fig 2. Microstructures of ekinFeCoNiAlgs alloy, a) SEM-ASE, b) TEM, ane (ouRTEM,_mierograpis given in ig. 2(b), which shows a single erystal superalloy like microstructure. The selected-area electron diffraction patterns (ig, 2001) and (62) indicated thatthe channel-shaped phase was BGC phase, while the cubicshaped phase was ordered B2 phase. The size of the cuboidal B2 phase was ranging from 100 to 300 nm, A coherent interface between the BCC and 82 phases was identified in the HR-TEM mage (Ss. 2(€). The lattice misfit (¢) between BCC end B2 was ‘calculated by the following formula asc a where the ang and apc isthe lattice parameter of B2 and BCC phase, respectively. In this work, aq anal ayce were measured from the HR-TEM pattems (/, 2(€) and which was 0.2905 nm and 0.2920 nm, respec tively. The lattice mismatch was calculated to be 0.53%, indicating thatthe coherent relationship between B2 and BCC phase. The composite structure of CrMaFeCoNtAlp73 alloy makes it possible to possess high strength and good ductility at elevated temperatures 25]. Superalloy. ike dual-phase microstructure has been reported in ‘many Al-containing HEAS, such as AlCuBeCiNip (x = 0.8-1.0) (26) AlCoCuCHFEN: [27,25], AlsCoCHFeNi (x = 0.5-0.9) [24], FesoNiaaMt inggAlis and PeasNiasMageAlzo [29], PegeMnaxCryeNhigAlso (0), and AlN, Co, Fe, Ces [81] In the AlpgCuFeCeNig (26), B2 (Ni-AL rich) ‘and BOG (Fe-Cr rich) were formed presumably vis spinodal decompo: sition. A multi-phase microstructure feature was also observed in ‘AlGoC+CuFeNi alloy, in which FCC, BCC, and B2 phases were detected 28], In addition, Wang et al, [2] systematically investigated the effect, ‘of Al addition on the erystal structure and microstructure of as-cast AlCoCe#eNi high-entropy alloy. They found that alloys containing low Al content had an FOC stricture and continuous increase of Al ‘content induced the formation of BCC phase which further spinodally ‘decomposed into modulated spinodal structure. The range ofx valve for ECC + BCC mixture was from near 0.5 (1.0 at % AD to 0.9 (18.4 2.9% ‘AD, Regarding whether FCC + B2 or BCG. + B2 phases are present inthe eNiMnAl alloys, Baker et al. (29) claimed that it depended on the ‘constituent elements that are the FCC or BCC phase stabilizer. Ma eta 91 also suggested that replacing strong FCC-sabilizing elements (Ni, Co) with BCC-stabilizing elements (Cr, Fe) or addition of other BCC stabilizes would increase the stability af the BCC phase in Alsi Co, Fe, COrsalay, In adaltion, the moderate ¢ of ~0.38% led tothe formation of coherent cuboidal B2 precipitate. For the present alloy CrMnFeCo [NiAlns, the Al content was 12.3 at%, and the contents of FCC phase stabilizer (Mn and Co) were relatively high (85.1 a9), Henee, the ‘observation of FCC + BCC/B2 multi-phase structure in CrMnFeCo INiAlors was reasonable and was consistent with the previous studies. 32. Chemical compositions of the phases and element distribution Chemical compositions of the FCC, BCC and 2 phases analyzed by “TEMLEDS were listed in Vble I. Iecould be seen that FCC phase was ‘composed of Cr, Fe, Co, Ma, and Ni. BCC phase had a composition (in atomic percent, a%) of 37.42 Cr, 28.87 Fe, 16.94 Co, 18.86 Mn, 2.20 INi,and 1.18 Al. The content of Cr (3.2 at.) and Fe (7.92 a4) was low while the content of Ni (36.17 a9) and Al (20.35 a.%) was high in B2 phase. Therefore, the BCC phase was a Cr-Fe rich phase while the B2 rete 1202020) 106744 phase was @ NLAI rich phase. The addition of AI into the single phase CCeMnFeCoNi was expected to introduce a large lattice distortion, and to promote the formation of FCC + BCC/B2 mult-phase structure [1]. AS the mixing enthalpy between Al and Ni is the most negative, as ‘compared to those between other constituent elements (Fable ?[22)), it fs favorable to the combination of land Ni during the alloy soidi- cation. The formation of NiAL-tich phase in the HEAs containing Ni and [Al were often observed inthe literature [19,21,23,29,30,39]. SD-APT was used to investigate the element distribution and the chemical composition in deeils for the eutectic-tike region shown in ig. 20), The elemental maps with different colors ofthe overall and individual atoms were shown in Fig. (0), indicated clearly that the distribution of constituent elements was non-uniform. Fe and Cr, Ni and AA elements could be divided into two regions based on the enrichment of constituent elements, whereas the distribution of Co and Mn was relatively homogeneous in two regions. A concentratlon-depth profile was plotted using a cylinder of a 10 « 10 nm? square oriented along the central Hine (ig. 5€0) through the analyzed volume. It i obvious from the concentration-lepth profile (°g. (¢) thatthe region on the top let comer (B2) was rich in Ni (~-40 at. 86) and Al(~20 a 6), suggesting that the B2 phase was @ NiAl-rieh phase, and the BCC phase was mainly ceariched in Fe (~30 at) and Cr (~'35 at. 99. The SD-APT result was ‘consistent with the TEM-EDS result 3.3. Compression mechanical properties "ig. 4 shows the compression stress-strain curves ofthe CrMnFeCo- NiAlo7s alloy tested from room-temperature to 900 °C. The room tem= perature yield strength and strain was 1194 MPa and 2.7%, respectively “Maccoscopicaly, she alloy exhibited atypical shear fracture made witha shearing angle of about 45°. AS observed in the inset of Fig. 4, the fracture morphology was mainly composed of farlike and river-like patterns, which were the typical fracture characteristics ofthe cleav- age fracture under compression. Moreover, some slip features caused by slip separation was also observed, due to the ductile fracture of FCC phase. The alloy showed an excellent combination of the strength and uctility at 400 °C and 500 °C, especially a noticeable increase in the compression strain. For example, at 500 °C, the alloy had a high yield strength (1070 MPa) and high compression strain (220%). Further in- crease in the testing temperature resulted in a decrease of the yield strength. The yield strength decreased significantly to about 600 MPa at {600 °C and the yield strength was only about 300 MPa at 700 °C. ‘ro understand the deformation mechanisms, TEM experiments were carried out for the samples deformed at room temperature, 400 °C, and 6600 °C, and the results were given in Ps. 5. Dislocations in the sample compressed at RF mainly pileup at the phase boundary between FCC and BCC ('e.5(@), indicating the motion of dislocations was impeded by the BCC regions, due tothe high strength of BCC compound itself. The igh volume fraction of the BCC phase could explain the high yield strength of 1194 MPa obtained at room temperature. At 400 °C, dislo- cations mainly distributed in the BCC phase. The distribution feature of dislocations was quite similar to rat in Uae conventional Ni-based su peralloys [34-36]. The strengthening effec of the ordered 82 phase can be mostly atributed to (i) small latice mist between the BCC and B2 phases (coherency strengthening); (i) the energy required to build Teble2 ‘rable ‘Atom radi of elements an the mila enthalples of etomleplis among ele Compositions of FOG, BEC ana 2 pases analyzed by TEMLEDS (at 6) sents mol 221 1c 19st m0) mai Res aal ara Ausicedwipe asa= eeReRseE Concentration (at. %) bee 0 5 0 1 2 2% 90 Distance (nm) Fig. 8, SD-APT result of CMnFeCoNiAlars aly. (a) The overall and indivi. ‘ual clement distribution ia an analyzed volume of 57 7 104 nm, b) and (© The one-dimensional concentration depth profiles of ll alloying clernents determined in lies witha volume of 10 x 10 x 30 nm antiphase boundaries and to move dislocations in an ordered structure (ordering strengthening) [95]. At 400 °C, the phase shape of B2 vas similar to Uhat at room temperature (i 5(b)), On the other hand, further increase in temperature to 600 °C, the phase size of B2 ‘decreased, a indicated by the arcows in ig. 5(0)- This may be caused by the cutting of dislocations in B2 phase at elevated temperatures. In rete 1202020) 106744 a3 3 Engineering stress (MPa) $8 8 ° 5 10 % 20 25 Engineering strain (%) Fig. 4. Compression engineering sresestain curves for GrMnFeCoNiAla 7s alloy a¢ room and elevated temperatures, The inset was fracture surface of CCAMMAFECONAl,y alloy at room temperature. ‘dition, dislocation climbing on B2 phase was also observed (he inset in Vig. 5(€), indicating the dislocation motion was sensitive to the temperature. Therefore, thermally activated dislocation motion in the alloy seems to easly oceur at temperature higher than 600 °C, For the sample deformed with larger stain (ie. 5(d), shearing of 82 phase by the slip bands could be seen. As such, the capability of B2 phase to {impede dislocation motion decreased with inereasing temperature, and hence the yield strength decreased significantly. Based on Fis. 5, the Schematics forthe dislocation behavior at room and elevated tempera- tures were draw and shown in Fg. 6. Atroom temperature and 400 °C, atthe frst stage of deformation, dislocations mainly existed in the FCC phase and pilearp atthe phase boundary between BOC and B2. Some slocations occasionally observed on 82 phase. At 600 °C, dislocations sheared the softened B2 phase and climbed on B2 phase. ‘The yield strength of FCC structured as-cast CeMnFeCoNi (7) and CCEMFeCONIAl,25 [35] as reported to be 188 MPa and 272 MPa, respectively. Compared tothe strength ofthese two alloys, CrMnFeCo- NiAlg7s showed much higher one. This could be attributed tothe for- ‘ation of ordered BCC/B2 phases in the alloy. It was reported that the yield strength of 82 phase isa temperature-dependence property [°° ‘The strength of B2 phase remains nearly constant level from room emperature to about 0.4 Tm (melting temperature), while It decreases pronouncedly at higher temperatures. The valu of 0 Ty forthe present alloy was estimated to be ~540 °C by the Therme-Cale software. Tis value is consisted with the observed preservation of high strength forthe present alloy a temperatures up to 500 °C. Hence, based on the above iscusson, the strengthening effect of B2 phase made the alloy possess high strength up to 500 °C, but the softening of B2 phase at and above 600 °C decreased the alloy strength ig. 7 compared the compression yield strengths of CeMaeCo- NiAlg7s alloy at different temperatures with several single or dual- phases HEAS (NoMoTaWT 6], FeieMna:CrisNiAlio [30], GrM{nFe CCoNI 10], and AICOCrCureNi (28) and Ni-base superalloy (Inconel 718 [1)) Ie could be seen that the compression strength of CrMneCo- NiAlazs alloy was very competitive among all the above-mentioned al- loys. The yield strength of CrMaFeCoNiAly7s alloy was 900 MPa higher than the typical CrMnFeCoN! slloy at temperature up t0 500 °C, indi cating thatthe addition of Al significantly enhanced the alloy strength. [At temperature up to 500 °C, which isthe common operating temper- ature for structural materials, the yield strength of CrMnFeCoNIAlnzs was similar to that ofthe superalloy Inconel 718. From the lo strength comparison results for CrMinFeCoNiAl 7s and the refractory NbMoTaW, we can find thatthe present alloy also showed advance in strength atrete 1202020) 106744 ns Fig. 5. TEM images ofthe CEMBPeCONiAlg alloy after compresion test ta) room temperature, b) 400°C, c) and 4) 600°C deformed with diferent sais. (a) RTand 400°C (b) 600°C dislocation confined in BCC & pile up dislocation shearing & climbing ig. 6, Schematics for deformation behavior ata) Rand 400 Cand b) 600 °C, temperature up to 600 °C ‘The strength comparison with the other alloys obviously shows that the CrMnFeCoNiAlo7s alloy was promising to be used as structur ‘materials, which required high strength up to 500 °C. Moreover, the allo fabricated withthe relatively cheap components makes the alloy ‘even more attractive for industry applications. In dation, as the alloy strength was obtained for the as-cast alloy, heat treatment and/or bot deformation processing can be used to optimize the microstructure and this may improve the mechanical properties of the alloy. 4. Conclusions (2) The CrMtaPeCoNiAlg7s was a multi-phase alloy, which consisted fof Fe-Ni-Co-Mn FCC phase, Cr-Fe-Co-Mn BCC phase and= é = £ 5 2 £ 2 = Se ee 0 200 400-600 Temperature (°C) 7. Comparison of yield strength for CAMNFECONAl.ys alloy and some alloys. Ni-AI-Co-Min B2 phase. The dual-phase region with Fine struc ture was composed of channelshaped BCC phase and cubic shaped B2 phase, ROC and B2 phases have small lattice mismatches. (2) The composite structure of CeMnFeCoNiAl7s alloy made it possess high strength up to 500 °C, Further increase inthe tem perature beyond 600 °C resulted in alloy softening (3) Thehigh strength was attributed tothe formation of high strength [BCC and ordered 82 phase inthe alloy, which effesvely impede the motion of dislocations below 600 °C. The decreased alloy strength at and above 600 °C may be due to the decrease in strength of B2 and BCC phase, dislocations cutting the B2 phase, and thermo-activated dislocation moverzent. Declaration of competing interest ‘We declare that we have no financial and personal relationships with ‘other people or organizations that can inappropriately influence our ‘work, there sno professional or other personal interest of any nature or {kind inany product, service and/or company that could be construed as influencing the position presented in, of the review of, the manuscript entitled. ‘CRediT authorship conteibution statement Lijing Lin: Writing - original draft, Data curation. Xin Xian: Writing original draft. Zhihong Zhong: Funding acquisition, Conceptuaiza ‘on, Writing - review & editing. Chang Chen: Methodology. Zhixiong ‘Zhu: Investigation, Yueheng Wut Methodology. Peter K, Liaw: Writing review & editing ‘Acknowledgments ‘he authors gratefully acknowledge the nancial support from the ‘National Natural Science Foundation of China (51401071, 51701056), the Natural Science Foundation of Anhu! Provice(1808085QF136), the National Magnetic Confinement Fusion Program of China (2015GB121003), and the Fundamental Research Funds for the Central Universities (PA20186DQ70018). References (1 2PM Wang MLN Che Bake, Ya C7 LT. Nh Anaennet| {nthe tre development of igeivgy ely: sammy fom eer Storksop, nets 6 218) 6727 hp so on Oy 2 o o ” ® » co) an a ns) on as) 8 an 08) 9) (23) an 251 (261 rete 1202020) 106744 DR Mal Seno Ac eve of gh oon aloe and ead ‘onc Ai Mate 12 (U7) HOST, hg eons Osa) DL Tn Yeh henropy alos: a reve, Mater. Res. Let. 22) {aove ton, peng a om, ees ne 3a 2hng TP, Tang, ME Can, KA abe, PR, 2b Duco nd pope of kino ly, rg Mate Sl 6 (2014) {5 enn, ih i. ale: Ch Chang, Law, Rey Beh Seton it, itera 180) 10) awe ee sone SY. cha, ¥ Tong KA Tan, JW. Yeh, 1D, pw, J Wen, KE Gan, Gh W Chen ¥. 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