Next Article in Journal
Seismic Performance Evaluation of RC Columns Retrofitted by 3D Textile Reinforced Mortars
Next Article in Special Issue
A Numerical Simulation Method Considering Solid Phase Transformation and the Experimental Verification of Ti6Al4V Titanium Alloy Sheet Welding Processes
Previous Article in Journal
Utilizing a Diffractive Focus Beam Shaper to Enhance Pattern Uniformity and Process Throughput during Direct Laser Interference Patterning
Previous Article in Special Issue
Texture Evolution during Recrystallization and Grain Growth in Non-Oriented Electrical Steel Produced by Compact Strip Production Process
 
 
Font Type:
Arial Georgia Verdana
Font Size:
Aa Aa Aa
Line Spacing:
Column Width:
Background:
Article

Experimental Investigation of the Phase Relations in the Fe-Zr-Y Ternary System

School of Material Science and Engineering, Central South University, Changsha 410083, China
*
Author to whom correspondence should be addressed.
Materials 2022, 15(2), 593; https://doi.org/10.3390/ma15020593
Submission received: 15 December 2021 / Revised: 5 January 2022 / Accepted: 11 January 2022 / Published: 13 January 2022
(This article belongs to the Special Issue Phase Structure and Functional Properties of Materials)

Abstract

:
The phase relations of the Fe-Zr-Y system at 973 K and 1073 K were experimentally investigated by using the equilibrated alloys. New ternary compounds τ3-Fe3ZrY and τ4-Fe10Zr5Y2 were found in this ternary system. The solubility of Y in Fe2Zr was measured to be 3.5 at.% and the third component can hardly dissolve in the other binary intermetallic phases. Experiments have verified that Fe2.9Zr0.5Y0.5 has a solid solubility ranging from Fe73Zr12Y14 to Fe77Zr9Y13.

1. Introduction

Due to the use of nuclear fusion and the third-generation nuclear fission reactors, zirconium-based alloys have been widely studied as important nuclear cladding materials [1,2,3,4,5]. This relies on their specific characteristics: excellent corrosion resistance, good mechanical properties, high resistance to radiation damage and a low cross section of capture for thermal neutrons [6]. The Fe-Zr-Y system is an important member of the zirconium-based nuclear cladding materials, the high temperature resistance and radiation resistance of which can be greatly improved after oxidation [7,8,9,10,11]. Although the Fe-Zr-Y system has excellent prospects, there are still some problems that limit its applications in industry. For example, when the temperature of a nuclear reactor core continuously rises, the Fe-Zr-Y system may be at risk of being unstable [12].
An efficient and effective solution to this problem is to obtain a comprehensive and profound understanding on phases of different components and rule out the phases that are unstable at high temperatures in advance. which is of vital importance for the applications of the Fe-Zr-Y system [13]. The purpose of this work is to explore the phase diagram of the Fe-Zr-Y system at high temperature in order to intuitively express the relationship between phases under the thermodynamic equilibrium state so as to provide a basic theoretical guide for the research, development, and design of new materials.
The experimental investigations on the phase relations of the Fe-Zr-Y system [14,15,16,17,18,19,20] have been carried out, and several assessments of thermodynamic data have been obtained [21,22,23,24,25,26]. Although there are some controversies about the stability of hex-Fe2Zr and Fe23Zr6, it is widely accepted that both of the two phases exist [3]. According to the results of X-ray and magnetic measurements, Kai et al. [27] confirmed the presence of hexagonal Fe2Zr, which had the same structure of MgNi2. Subsequently, Stein et al. [28] found the Fe2Zr phase of C36-type structure through heat treatment at 1563 K. Meanwhile, Liu et al. [16] confirmed the existence of Fe23Zr6 by using a transmission electron microscope (TEM) and a scanning transmission electron microscope (STEM). Recently, Yang et al. [29] and Lu et al. [30] applied first-principles calculations to evaluate the formation enthalpy of compounds in Fe-Zr system, in which Fe23Zr6 was considered as a stable phase. After a thorough survey and thermodynamic evaluations based on a number of experiments, the binary phase diagrams reported by Lu et al. [30] were finally adopted in this work. As shown in Figure 1, among the four intermetallic phases, only Fe2Zr phase has an obvious homogeneity range. In other phases, FeZr2 appears in the temperature range of 1215–1054 K, and FeZr3 is formed through peritectoid reaction.
Domagala et al. [31] reported the Fe-Y phase diagram for the first time in the whole composition range. Then, a thermodynamic assessment was carried out by Gschneider et al. [32] Recently, Zhang et al. studied the crystallography and thermodynamics of the compounds in the system, which provided a basis for further optimization of the Fe-Y system [33]. Figure 2 shows the Fe-Y phase diagram with four intermetallic compounds: Fe17Y2, Fe23Y6, Fe3Y and Fe2Y. Based on the previous research work mentioned above, Saenko et al. [34] reported the thermodynamic optimization of the Fe-Y binary system, as shown in Figure 2.
The phase equilibrium relation of Zr-Y phase diagram was first studied by Wang [35], based on which Palenzona and Ciraflci [36] optimized the thermodynamic data. Recently, Flandorfer et al. [37] constructed the thermodynamic database of Zr-Y system. The calculated phase diagram used in this work adopts the latest thermodynamic parameters reported by Bu et al. [38], as shown in Figure 3.
Research on the phase relationships and ternary compounds of Fe-Zr-Y ternary systems was relatively limited. In 1986, by combining three related binary phase diagrams, Harchenko et al. [39] measured the 1070K isothermal section of the Fe-Zr-Y ternary system for the first time, but no ternary compounds were discovered, as shown in Figure 4. In 1989, Jifan et al. reported Fe9Zr2Y phase with ThMn12 structure [40]. At the same time, Itoh et al. also found Fe2.9Zr0.5Y0.5 phase of Orthorhombic type [41]. The binary and ternary phases, the crystal structure and lattice parameters that were previously reported are listed in Table 1.

2. Experimental Procedures

The phase relationship of the Fe-Zr-Y system was studied through the equilibrium alloy method of static measurements. Iron rod (99.99 wt.%), zirconium rod (99.99 wt.%) and yttrium block (99.99 wt.%) were selected as raw materials. The weight of the samples was controlled around 12 g, with an error of ±0.005 g. The samples were placed in a non-expendable arc melting furnace with high purity argon atmosphere. At the same time, a sponge titanium button was added as the oxygen absorber to prevent oxidation. Each alloy button was melted for at least 4 times to ensure its uniformity. The alloy buttons were divided into two parts and sealed in the quartz tubes filled with argon. According to the reported heat treatment processes of similar systems [3], 60 and 90 days were set as the annealing times for 700 °C and 800 °C, respectively. After annealing, the samples were quenched in cold water to preserve the microstructure at high temperature.
The morphology and phase compositions of the alloy were analyzed by electron probe microanalysis (EPMA, JAXA-8800R, JEOL, 15 kV, 1 × 10−8 A, Tokyo, Japan). X-ray diffraction was employed (XRD, Rigaku d-max/2550 VB, Cu K, 40 kV, 250 mA, Tokyo, Japan) to analyze the crystal structure of typical alloys, with the scanning range of 10–90° and a speed of 0.133°/s. Backscattering electron (BSE) images of the alloy samples were acquired using a scanning electron microscope (SEM, TESCAN MIRA3 LMH, 15 kV, working distance of 15 mm, Brno, The Czech Republic).

3. Experimental Results

Based on the phase equilibrium data of 24 alloy samples, the isothermal section of the Fe-Zr-Y ternary system at 973 K was determined for the first time, as shown in Figure 5. A total of 12 three-phase regions and 12 two-phase regions were measured. In this isothermal section, there are four ternary compounds, among which, τ1, τ3 and τ4 have solid solubility intervals, and seven binary compounds, three of which have solid solubility, which are Fe2Zr, FeZr3, Fe2Y.
The isothermal section of Fe-Zr-Y ternary system at 1073 K is similar to the system at 973 K except that the maximum solid solubility of compounds τ1 and τ3 are slightly higher at 1073 K. Additionally, FeZr2 as a high temperature phase appeared at 1073 K. This is consistent with the binary optimized phase diagram, and therefore its appearance is reasonable and in accordance with expectation [30]. The 1073 K isothermal section obtained in this work is shown in Figure 6.

4. Discussion

The experimental data obtained from SEM, EPMA, XRD and EBSD examination were analyzed to determine the isothermal section and the phase relationship of the Fe-Zr-Y ternary system at 973 K and 1073 K. The phase relations in several key alloys were discussed in detail as follows.

4.1. Phase Equilibria at 973 K

A total of 24 alloy samples were prepared for the study of the phase equilibria of the Fe-Zr-Y ternary system at 973 K. The constituent phases of each alloy sample were summarized in Table 2.
BSE images and XRD patterns of alloy samples A7, A13 and A24 are shown in Figure 7a,c,e). EPMA-WDS results show that the dark gray phases in A7, A13 and A24 have the same composition, close to Fe60Zr20Y20, so they are confirmed as the same phase. However, this composition is different from the existing ternary compounds in the Fe-Zr-Y system. For the further identification of this phase, XRD analysis was performed on all three samples. In the XRD patterns of the three alloys, there are unrecorded characteristic peaks, the positions of which are basically fixed. Only a few peaks have slight displacement, which may be due to the change in lattice parameters. According to the above analysis, the ternary compound was identified as a new phase with the chemical formula Fe3ZrY and named τ3. Since no single phase of τ3 was obtained in this work, follow-up experiments are needed to explore the crystal structure of τ3.
There are three phases in the BSE images of alloy samples A2 and A9 (Figure 8a,c). According to the results of XRD and EPMA-WDS tests, all the phases are already identified except for the black phase. The compositions of the black phase in Figure 8a,c are Fe59.7Zr29.6Y10.5 and Fe56.2Zr27.9Y15.9, respectively. The stoichiometric ratios represent some differences between the two compositions, so the black phase was initially considered to be two different compounds. However, the XRD patterns (Figure 8b,d) show that the characteristic peaks of the two matched up, indicating that the crystal structures of the two phases were consistent, thus the two phases were confirmed to be the same compound. No ternary compound with similar stoichiometric ratio and diffraction peak matching was found in PDF cards. According to the results described above, the black phase was defined as the new ternary compound Fe10Zr5Y2 and named as τ4.
The BSE images of alloy samples A5, A10 and A17 are shown in Figure 9a,c,e. The black phase in A10 and the dark gray phase in A5 and A17 have the same atomic ratio of Fe2.9Zr0.5Y0.5, which was denoted as τ1 phase. The XRD (as shown in Figure 9b,d,f) characteristic peaks of compound τ1 have fixed positions, which are different from all the existing PDF cards. According to the reported literature [41], Fe2.9Zr0.5Y0.5 was considered to be transformed from Fe3Y, as Zr atoms replaced Y atoms in Fe3Y. In the study of Itoh et al. [41], Fe3Y did not exist in the Fe-Zr-Y system, as it was considered to be present in the form of Fe2.9ZrxY1−x (0 ≤ x ≤ 1), meaning that Y would be replaced by Zr until Y disappears completely. This conclusion was not adopted in this work due to the following reasons: (1) Fe2.9Zr0.5Y0.5 would be adjacent to Fe3Y phase according to the reported theory [41], which is not consistent with what is shown in Figure 9a,c,e. Although there is Fe3Y shown in Figure 9c, it is separated by Fe23Y6, and τ1 is completely wrapped by Fe23Y6 instead of Fe3Y. (2) If Fe2.9ZrxY1−x (0 ≤ x ≤1) phase exists, the solubility range of Zr in Fe3Y would pass through most of the phase equilibrium region, which violates the law of phase equilibrium relation. In conclusion, the phase Fe2.9ZrxY1−x (0 ≤ x ≤ 1) is not adopted in this work.
BSE image Figure 10a illustrates the phase composition in alloy A4, which is composed of three phases. The results of EPMA-WDS show the continuously distributed matrix phase and the gray phase had the composition of Fe68.1Zr29.3Y2.6 and Fe88.2Y11.8, and were, respectively, determined as Fe2Zr and Fe17Y2 according to the XRD results of Figure 10b. The black phase labeled τ2 was presumed to be an unknown ternary compound at first, because the diffraction peaks cannot be matched by any PDF card corresponding to the crystal structure of the stable solid phase in the ternary system. However, they are indexed by a ThMn12 type crystal structure and obtain the characteristic peaks of Fe9Zr2Y, which coincide with τ2 in the literature [40]. Therefore, τ2 phase was finally identified as the ternary compound Fe9Zr2Y.
Figure 11 shows the BSE images and XRD patterns of A16 and A18. According to the data from EPMA-WDS, the maximum atomic percentage of Zr in Fe2Zr is 37.6 at 973 K in A16. Combining Figure 11c with Figure 5, it can be seen that Y tends to precipitate in the form of metal simple substance most of the time, which is in accord with the results obtained by Nouri et al. [38] Meanwhile, Y phase is dispersed, indented and porous, which can be mainly ascribed to the result of rapid galvanic corrosion of the (Y), which acts as anode with Continuous-distributed matrix as cathode during polishing (or exposure to the moisture) [38].

4.2. Phase Equilibria at 1073 K

The phase equilibrium of the Fe-Zr-Y ternary system at 1073 K was also investigated in this work. A total of 25 alloy samples were annealed at 1073 K for 60 days. The phases and compositions of each alloy are listed in Table 3.
With the increase in temperature, the solid solubility region of τ1 and Fe2Zr becomes larger, and a new high temperature phase FeZr2 appears. This result is consistent with the binary phase diagram of Fe-Zr, but the exact formation temperature of FeZr2 had not been reported to date. The XRD pattern of B23 in Figure 12b shows the same characteristic peaks of FeZr2 as standard PDF cards. Combined with EPMA-WDS data, it can be seen that the dark phase in BSE image Figure 12a is the binary compound FeZr2.

5. Conclusions

In this work, the phase relationship of the Fe-Zr-Y ternary system at 973 K and 1073 K combined with EPMA-EDS, XRD and SEM results was studied systematically. There are twelve and thirteen three-phase regions measured at 973 K and 1073 K, respectively. At 1073 K, the solution ranges of τ1-Fe2.9Zr0.5Y0.5 are from Fe73Zr12Y14 to Fe77Zr9Y13. The maximum solid solubility of Y in Fe2Zr is 4 at.% and atomic ratio of Fe2Zr is from Fe62Zr38 to Fe71Zr29 at 1073 K. New ternary compounds τ3-Fe3ZrY and τ4-Fe10Zr5Y2 were investigated. Those isothermal sections at 1073 K and 973 K provide the possibility of providing a thermodynamic description of the system through the CALPHAD method, allowing more reliable extrapolations of the Fe-Zr-Y system to be used in the nuclear industry.

Author Contributions

Conceptualization, L.Z. and C.L.; methodology, X.Y.; software, Q.H.; validation, Y.W.; formal analysis, C.L. and X.Y.; investigation, C.L. and Q.S.; resources, Q.S. and Q.H.; data curation, C.L.; writing—original draft preparation, Q.S.; writing—review and editing, C.L.; visualization, L.L.; supervision, L.Z.; project administration, L.Z.; funding acquisition, L.Z. All authors have read and agreed to the published version of the manuscript.

Funding

The work was financially supported by National MCF Energy R&D Program of China (No. 2018YFE0306100), National Natural Science Foundation of China (No. 51871248) and Natural Science Foundation of Hunan Province, China (No. 2020JJ4739).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Not applicable.

Conflicts of Interest

The authors declare no conflict of interest.

References

  1. Celbová, L.; Ashcheulov, P.; Klimša, L.; Kopeček, J.; Dragounová, K.A.; Luštinec, J.; Macák, J.; Škoda, R.; Kratochvílová, I. Diamond Coating Reduces Nuclear Fuel Rod Corrosion at Accidental Temperatures: The Role of Surface Electrochemistry and Semiconductivity. Materials 2021, 14, 6315. [Google Scholar] [CrossRef]
  2. Diniasi, D.; Golgovici, F.; Marin, A.H.; Negrea, A.D.; Fulger, M.; Demetrescu, I. Long-Term Corrosion Testing of Zy-4 in a LiOH Solution under High Pressure and Temperature Conditions. Materials 2021, 14, 4586. [Google Scholar] [CrossRef]
  3. Zou, N.; Lu, H.-J.; Liu, L.-L.; He, Y.-L.; Lu, X.-G. Experimental investigation of phase equilibria in the Fe-Hf-Zr system at 1173 K and 1373 K. Calphad 2021, 72, 102240. [Google Scholar] [CrossRef]
  4. Zhang, H.; Du, Y.; Shen, Z.; Zhou, P.; Peng, Y.; Liu, S.; Kong, Y.; Rajkumar, V.B. Thermodynamic modeling and solidified microstructure in the Mo–Nb–Zr ternary system. Calphad 2019, 66, 101630. [Google Scholar] [CrossRef]
  5. Zeng, Y.; Zhou, P.; Du, Y.; Mo, W.; Bai, B.; Wang, X.; Zhao, J. A thermodynamic description of the U−Ti−Zr system. Calphad 2018, 60, 90–97. [Google Scholar] [CrossRef]
  6. Nieva, N.; Corvalán, C.; Jiménez, M.J.; Gómez, A.; Arreguez, C.; Joubert, J.M.; Arias, D. Phase diagram of the Fe-Sn-Zr system at 800 °C. J. Nucl. Mater. 2017, 487, 186–191. [Google Scholar] [CrossRef]
  7. Wang, Y.; Xu, S.; Jia, H.; Tong, Z.; Zhou, Z. Influence of Zr addition on the microstructure and mechanical properties of 9CrTi-ODS steels. Nucl. Mater. Energy 2021, 29, 101101. [Google Scholar] [CrossRef]
  8. Gómez-Acebo, T. Summary report of CALPHAD XLII—San Sebastian, Spain, 2013. Calphad 2014, 45, 62–117. [Google Scholar] [CrossRef]
  9. Li, Z.; Chen, L.; Zhang, H.; Liu, S. High-Temperature Oxidation Properties and Microstructural Evolution of Nanostructure Fe-Cr-Al ODS Alloys. Materials 2021, 14, 526. [Google Scholar] [CrossRef]
  10. Zhou, X.; Li, G.; Shen, X.; Liu, Y. Tensile strength improvement of martensitic ODS steels with Zr and Hf additions. Mater. Sci. Eng. A 2022, 829, 142071. [Google Scholar] [CrossRef]
  11. Peng, S.; Lu, Z.; Yu, L. Effects of Y2O3/Ti/Zr addition on microstructure and hardness of ODS-CoCrFeNi HEAs produced by mechanical alloying and spark plasma sintering. J. Alloys Compd. 2021, 861, 157940. [Google Scholar] [CrossRef]
  12. Chang, K.-C.; Zhao, J.-R.; Hung, F.-Y. Effects of hyper-high-temperature solid-solution treatment on microstructure evolution and nanoprecipitation of the Al-Ni-Cu-Fe-Zr-Sc alloy manufactured by selective laser melting. J. Alloys Compd. 2021, 883, 160781. [Google Scholar] [CrossRef]
  13. Sundman, B.; Dupin, N.; Hallstedt, B. Algorithms useful for calculating multi-component equilibria, phase diagrams and other kinds of diagrams. Calphad 2021, 75, 102330. [Google Scholar] [CrossRef]
  14. Malakhova, T.; Alekseyeva, Z. The Zr-Fe phase diagram in the range 20–40 at.% Fe and the crystalline structure of the intermetallic compound Zr3Fe. J. Less Common Met. 1981, 81, 293–300. [Google Scholar] [CrossRef]
  15. Raghavan, V. Al-Fe-Zr (Aluminum-Iron-Zirconium). J. Phase Equilibria Diffus. 2010, 31, 459–462. [Google Scholar] [CrossRef]
  16. Liu, Y.; Allen, S.M.; Livingson, J.D. An investigation of Fe3Zr phase. Scr. Metall. Mater. 1995, 32, 1129–1132. [Google Scholar] [CrossRef]
  17. Granovsky, M.S.; Canay, M.; Lena, E.; Arias, D. Experimental investigation of the Zr corner of theternary Zr–Nb–Fe phase diagram. J. Nucl. Mater. 2002, 302, 1–8. [Google Scholar] [CrossRef]
  18. Zeng, L.; Xu, G.; Liu, L.; Bai, W.; Zhang, L. Experimental investigation of phase equilibria in the Ti-Fe-Zr system. Calphad 2018, 61, 20–32. [Google Scholar] [CrossRef]
  19. Ye, J.; Guan, R.; Zhao, H.; He, C.; Xiong, K. Effect of Zr Microalloying on the Microstructures and Strengthening Mechanism of As-Cast Al-Fe-Zr Alloys. Materials 2020, 13, 4744. [Google Scholar] [CrossRef]
  20. Malakhova, T.O.; Kobylkin, A.N. Phase diagram for Zr-Fe(0-66,6 at.%Fe). Izvestiya Akademii Nauk SSSR Metally 1982, 14, 205–209. [Google Scholar]
  21. Servant, C.; Gueneau, C.; Ansara, I. Experimental and thermodynamic assessment of the Fe-Zr system. J. Alloys Compd. 1995, 220, 19–26. [Google Scholar] [CrossRef]
  22. Saenko, I.; Kuprava, A.; Udovsky, A.; Fabrichnaya, O. Heat capacity measurement of Zr2Fe and thermodynamic re-assessment of the Fe–Zr system. Calphad 2019, 66, 101625. [Google Scholar] [CrossRef]
  23. Jiang, M.; Oikawa, K.; Ikeshoji, T.; Wulff, L.; Ishida, K. Thermodynamic Calculations of Fe-Zr and Fe-Zr-C Systems. J. Phase Equilibria Diffus. 2000, 22, 406–417. [Google Scholar] [CrossRef]
  24. Zou, N.; Lu, H.-J.; Gu, P.-W.; Wang, J.-Y.; Feng, X.-K.; Shen, J.-Y.; He, Y.-L.; Li, L.; Lu, X.-G. Thermodynamic assessment and glass forming ability prediction of the Zr-Fe-Cu system. Calphad 2019, 64, 175–184. [Google Scholar] [CrossRef]
  25. Rigaud, V.; Sundman, B.; Daloz, D.; Lesoult, G. Thermodynamic assessment of the Fe–Al–Zr phase diagram. Calphad 2009, 33, 442–449. [Google Scholar] [CrossRef]
  26. Cui, J.; Shen, Y.; Liu, X. Experimental investigation and thermodynamic modeling of the Fe−Si−Zr system. Calphad 2019, 65, 385–401. [Google Scholar] [CrossRef]
  27. Kai, K.; Nakamichi, T.; Yamamoto, M. Crystal Structures and Magnetic Properties of the Intermetallic Compnd Fe2Zr. J. Phys. Soc. 1968, 25, 1192. [Google Scholar] [CrossRef]
  28. Stein, F.; Sauthoff, G.; Palm, M. Experimental Determination of Intermetallic Phases, Phase Equilibria, and Invariant Reaction Temperatures in the Fe-Zr System. J. Phase Equilibria Diffus. 2002, 23, 480–494. [Google Scholar] [CrossRef]
  29. Yang, Y.; Tan, L.; Bei, H.; Busby, J.T. Thermodynamic modeling and experimental study of the Fe–Cr–Zr system. J. Nucl. Mater. 2013, 441, 190–202. [Google Scholar] [CrossRef]
  30. Lu, H.-J.; Zou, N.; Zhao, X.-S.; Shen, J.-Y.; Lu, X.-G.; He, Y.-L. Thermodynamic investigation of the Zr-Fe-Nb system and its applications. Intermetallics 2017, 88, 91–100. [Google Scholar] [CrossRef]
  31. Domagala, R.F.; Rausch, J.J.; Levinson, D.W. The systems Y-Fe, Y-Ni, and Y-Cu. Trans. Am. Soc. Met. 1961, 53, 139–155. [Google Scholar]
  32. Gschneidner, K.A., Jr. Rare Earth Alloys; D. Van Nostrand Company Inc.: Princeton, NJ, USA, 1961; Volume 60, p. 247. [Google Scholar]
  33. Zhang, W.; Liu, G.; Han, K. The Fe-Y (iron-yttrium) system. J. Phase Equilibria 1992, 13, 304–308. [Google Scholar] [CrossRef]
  34. Saenko, I.; Fabrichnaya, O.; Udovsky, A. New Thermodynamic Assessment of the Fe-Y System. J. Phase Equilibria Diffus. 2017, 38, 684–699. [Google Scholar] [CrossRef]
  35. Wang, R. Formation of metastable low temperature allotropie solid solutions in rare earth-zirconium systems. Metall. Trans. 1972, 3, 1213–1221. [Google Scholar] [CrossRef]
  36. Palenzona, A.; Cirafici, S. The Y-Zr (yttrium-zirconium) system. J. Phase Equilibria 1991, 12, 485–489. [Google Scholar] [CrossRef]
  37. Flandorfer, H.; Gröbner, J.; Stamou, A.; Hassiotis, N.; Saccone, A.; Rogl, P.; Wouters, R.; Seifert, H.; Macciò, D.; Ferro, R. Experimental investigation and thermodynamic calculation of the ternary system Mn–Y–Zr. Int. J. Mater. Res. 1997, 88, 529–538. [Google Scholar]
  38. Bu, M.J.; Wang, P.S.; Xu, H.H.; Liu, S.H.; Sha, C.S.; Du, Y.; Pan, F.S.; Tang, A.T. Experimental investigation and thermodynamic modeling of the Zr-Y system. J. Min. Metall. Sect. B Metall. 2010, 46, 181–192. [Google Scholar] [CrossRef]
  39. Harchenko, O.I.; Berezyuk, D.A.; Kryshtal, M.I. Ternary (Y,Ce)-Zr-Fe systems. Visn. L'vivs'kogo (Derzhavnogo) Univ. Seriya Khimichna 1984, 25, 26–28. [Google Scholar]
  40. Jifan, H.; Mingxi, L.; Rufeng, X.; Shougong, Z.; Zhenxi, W. Formation of Magnetic Phases in Y-Zr-Fe Compounds. Phys. Stat. Sol. 1989, 113, 127–129. [Google Scholar]
  41. Itoh, K.; Okagaki, T.; Kanematsu, K. Crystal Structure and Magnetic Properties of Y1-xZrxFe2.9. J. Phys. Soc. 1989, 58, 1787–1792. [Google Scholar] [CrossRef]
  42. Villars, P. Pearson’s Handbook Desk Edition: C. Data for Intermetallic Phases, volume 2. ASM Int. 1997, 1, 1143. [Google Scholar]
  43. Nouri, K.; Jemmali, M.; Walha, S.; Salah, A.B.; Dhahri, E.; Bessais, L. Experimental investigation of the Y-Fe-Ga ternary phase diagram: Phase equilibria and new isothermal section at 800 °C. J. Alloys Compd. 2017, 719, 256–263. [Google Scholar] [CrossRef]
Figure 1. The calculated Fe-Zr phase diagram based on the work of Lu et al. [30].
Figure 1. The calculated Fe-Zr phase diagram based on the work of Lu et al. [30].
Materials 15 00593 g001
Figure 2. The calculated Fe-Y phase diagram based on the work of Saenko et al. [34].
Figure 2. The calculated Fe-Y phase diagram based on the work of Saenko et al. [34].
Materials 15 00593 g002
Figure 3. The calculated Y-Zr phase diagram based on the work of Bu et al. [38].
Figure 3. The calculated Y-Zr phase diagram based on the work of Bu et al. [38].
Materials 15 00593 g003
Figure 4. The 1070K isothermal section of the Fe-Zr-Y ternary system [39].
Figure 4. The 1070K isothermal section of the Fe-Zr-Y ternary system [39].
Materials 15 00593 g004
Figure 5. Isothermal section of the Fe-Zr-Y ternary system at 973 K determined in this work.
Figure 5. Isothermal section of the Fe-Zr-Y ternary system at 973 K determined in this work.
Materials 15 00593 g005
Figure 6. Isothermal section of the Fe-Zr-Y ternary system at 1073 K obtained in this work.
Figure 6. Isothermal section of the Fe-Zr-Y ternary system at 1073 K obtained in this work.
Materials 15 00593 g006
Figure 7. (a) BSE image of A13 (b) XRD pattern of A13 (c) BSE image of A1 of A24 (d) XRD pattern of A24 (e) BSE image of A7 (f) XRD pattern of A7.
Figure 7. (a) BSE image of A13 (b) XRD pattern of A13 (c) BSE image of A1 of A24 (d) XRD pattern of A24 (e) BSE image of A7 (f) XRD pattern of A7.
Materials 15 00593 g007
Figure 8. (a) BSE image of A2 (b) XRD pattern of A2 (c) BSE image of A9 (d) XRD pattern of A9.
Figure 8. (a) BSE image of A2 (b) XRD pattern of A2 (c) BSE image of A9 (d) XRD pattern of A9.
Materials 15 00593 g008
Figure 9. (a) BSE image of A5 (b) XRD pattern of A5 (c) BSE image of A17 (d) XRD pattern of A17 (e) BSE image of A10 (f) XRD pattern of A10.
Figure 9. (a) BSE image of A5 (b) XRD pattern of A5 (c) BSE image of A17 (d) XRD pattern of A17 (e) BSE image of A10 (f) XRD pattern of A10.
Materials 15 00593 g009
Figure 10. (a) BSE image of A4 (b) XRD pattern of A4.
Figure 10. (a) BSE image of A4 (b) XRD pattern of A4.
Materials 15 00593 g010
Figure 11. (a) BSE image of A16 (b) XRD pattern of A16 (c) BSE image of A18 (d) XRD pattern of A18.
Figure 11. (a) BSE image of A16 (b) XRD pattern of A16 (c) BSE image of A18 (d) XRD pattern of A18.
Materials 15 00593 g011
Figure 12. (a) BSE image of B23 (b) XRD pattern of B23.
Figure 12. (a) BSE image of B23 (b) XRD pattern of B23.
Materials 15 00593 g012
Table 1. Experimental and literature data on crystal structures and lattice parameters of the solid phases in the Fe-Zr-Y system.
Table 1. Experimental and literature data on crystal structures and lattice parameters of the solid phases in the Fe-Zr-Y system.
PhasePhase
Prototype
Space Group Lattice Parameters (nm) Reference
abc
α (Fe)W Im 3 ¯ m0.29315//[42]
δ (Fe)W Im 3 ¯ m0.29315//[42]
β (Zr)W Im 3 ¯ m0.3568//[42]
γ (Fe)Cu Fm 3 ¯ m0.36599//[42]
α (Zr)MgP63/mmc0.323178/0.514831[28]
Fe2Zr_C15MgCu2 Fd 3 ¯ m0.702//[28]
Fe23Zr6Mn23Th6 Fm 3 ¯ m1.172//[28]
FeZr2Al2CuI4/mcm0.638/0.56[28]
FeZr3BRe3Cmcm0.3321.10.882[28]
Fe17Y2Th2Zn17 R 3 ¯ m0.846/1.241[43]
Fe23Y6Th6Mn23 Fm 3 ¯ m1.2082//[43]
Fe3YPuNi3 R 3 ¯ m0.515/2.46[43]
Fe2YMgCu2 Fd 3 ¯ m7.363//[43]
Fe9Zr2YThMn12I4/mmm0.86620.86620.50226[40]
Fe2.9Zr0.5Y0.5//0.50670.86342.451[41]
Table 2. Constituent phases and compositions in the annealed Fe-Zr-Y alloys at 973 K for 90 days.
Table 2. Constituent phases and compositions in the annealed Fe-Zr-Y alloys at 973 K for 90 days.
Alloy
(No.)
Chemical
Composition
Nominal Composition (at.%)Experimental Results (at.%)Phase
Determination
FeZrYFeZrY
A1Fe10Zr70Y2010702062.6137.230.16Fe2Zr
24.3574.421.23FeZr3
0.290.1399.58Y
A2Fe60Zr30Y1060301059.2224.4616.32τ3
59.7729.6110.62τ4
65.8531.842.31Fe2Zr
A3Fe10Zr60Y3010603023.3175.161.53FeZr3
2.8195.821.37Zr
98.870.150.98Y
A4Fe77Zr16Y77716768.1429.312.55Fe2Zr
75.8116.128.07τ2
88.240.2111.55Fe17Y2
A5Fe80Zr4Y168041675.4910.1214.39τ1
78.740.2820.98Fe23Y6
88.260.1711.57Fe17Y2
A6Fe45Zr20Y3545203557.3423.8918.77τ3
56.5427.7515.71τ4
0.210.1699.63Y
A7Fe50Zr10Y4050104059.1421.319.56τ3
99.540.160.30Y
65.353.3431.31Fe2Y
A8Fe65Zr20Y1565201565.8631.842.30Fe2Zr
61.1122.5416.35τ3
65.383.3631.26Fe2Y
A9Fe55Zr30Y1555301562.5135.482.01Fe2Zr
57.1729.613.23τ4
0.110.2599.64Y
A10Fe70Zr15Y1570151574.6211.7713.61τ1
65.342.7431.92Fe2Y
66.5430.862.60Fe2Zr
A11Fe62Zr32Y66232665.1333.111.76Fe2Zr
59.3530.3610.29τ4
A12Fe20Zr60Y202060200.150.2499.61Y
23.5974.421.99FeZr3
A13Fe61Zr25Y1461251459.4424.4216.14τ3
65.8731.822.31Fe2Zr
A14FeZr74Y25174251.5296.931.55Zr
0.140.1899.68Y
A15Fe15Zr84Y158411.1995.922.89Zr
23.2175.960.83FeZr3
A16Fe29Zr70Y2970124.3374.411.26FeZr3
62.4537.440.11Fe2Zr
A17Fe75Zr6Y197561974.719.6915.6τ1
75.330.2524.42Fe3Y
78.750.3320.92Fe23Y6
A18Fe55Zr30Y1555301562.3135.871.82Fe2Zr
0.340.1399.53Y
A19Fe50Zr25Y2550252556.2527.9115.84τ4
0.210.1199.68Y
A20Fe39ZrY603916065.451.8632.69Fe2Y
0.240.2399.53Y
A21Fe70ZrY297012966.870.1632.97Fe2Y
73.410.5426.05Fe3Y
A22Fe66Zr10Y2466102465.662.7431.6Fe2Y
66.3530.822.83Fe2Zr
A23Fe4Zr8Y88488880.3319.370.30Fe23Zr6
88.210.1511.64Fe17Y2
98.560.740.70Fe
A24Fe60Zr18Y2260182265.393.1831.43Fe2Y
60.2521.2418.51τ3
Table 3. Constituent phases and compositions in the annealed Fe-Zr-Y alloys at 1073 K for 60 days.
Table 3. Constituent phases and compositions in the annealed Fe-Zr-Y alloys at 1073 K for 60 days.
Alloy
(No.)
Chemical
Composition
Nominal Composition (at.%)Experimental Results (at.%)Phase
Determination
FeZrYFeZrY
B1Fe10Zr70Y2010702062.2137.720.07Fe2Zr
31.7267.370.91FeZr2
0.130.2199.66Y
B2Fe60Zr30Y1060301059.2524.4116.34τ3
59.7329.6610.61τ4
65.4231.213.37Fe2Zr
B3Fe10Zr60Y3010603024.3474.481.18FeZr3
93.863.842.3Zr
0.350.1399.52Y
B4Fe77Zr16Y77716768.1529.332.52Fe2Zr
75.8416.177.99τ2
88.250.1611.59Fe17Y2
B5Fe80Zr4Y168041677.489.5912.93τ1
78.770.2720.96Fe23Y6
88.220.1511.63Fe17Y2
B6Fe45Zr20Y3545203557.6322.7419.63τ3
56.5427.7015.76τ4
0.120.2599.63Y
B7Fe50Zr10Y4050104058.2920.0121.7τ3
0.350.1699.49Y
65.313.3631.33Fe2Y
B8Fe65Zr20Y1565201565.4731.283.25Fe2Zr
60.5521.1618.29τ3
65.3412.6122.05Fe2Y
B9Fe55Zr30Y1555301561.8934.823.29Fe2Zr
56.6828.814.52τ4
0.510.2099.29Y
B10Fe70Zr15Y1570151573.1412.4814.38τ1
65.332.7131.96Fe2Y
66.5930.652.76Fe2Zr
B11Fe62Zr32Y66232663.2332.454.32Fe2Zr
10.2830.7958.93τ4
B12Fe20Zr60Y202060200.410.3899.21Y
1.7375.223.07FeZr3
B13Fe61Zr25Y1461251460.1723.1216.71τ3
65.5431.353.11Fe2Zr
B14FeZr74Y25174251.8196.551.64Zr
0.150.2599.6Y
B15Fe15Zr84Y158410.8794.834.3Zr
22.6176.520.87FeZr3
B16Fe29Zr70Y2970124.4574.890.66FeZr3
31.3168.610.08FeZr2
B17Fe75Zr6Y197561975.749.5714.69τ1
75.310.3624.33Fe3Y
77.510.8521.64Fe23Y6
B18Fe55Zr30Y1555301561.9436.131.93Fe2Zr
0.100.2199.69Y
B19Fe50Zr25Y2550252556.2428.2915.47τ4
0.320.1599.53Y
B20Fe39ZrY603916065.411.8132.78Fe2Y
0.140.3299.54Y
B21Fe70ZrY297012966.9632.520.52Fe2Y
75.060.1024.84Fe3Y
B22Fe66Zr10Y2466102465.543.3631.1Fe2Y
66.1130.912.98Fe2Zr
B23Fe20Zr60Y2020602022.9575.471.58FeZr3
0.130.1399.74Y
31.2068.640.16FeZr2
B24Fe84.5Zr12.5Y384.512.5380.3119.610.08Fe23Zr6
88.870.8310.3Fe17Y2
99.150.170.68Fe
B25Fe60Zr18Y2260182265.323.3731.31Fe2Y
59.2120.2920.5τ3
Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Share and Cite

MDPI and ACS Style

Li, C.; Song, Q.; Yang, X.; Wei, Y.; Hu, Q.; Liu, L.; Zhang, L. Experimental Investigation of the Phase Relations in the Fe-Zr-Y Ternary System. Materials 2022, 15, 593. https://doi.org/10.3390/ma15020593

AMA Style

Li C, Song Q, Yang X, Wei Y, Hu Q, Liu L, Zhang L. Experimental Investigation of the Phase Relations in the Fe-Zr-Y Ternary System. Materials. 2022; 15(2):593. https://doi.org/10.3390/ma15020593

Chicago/Turabian Style

Li, Chenbo, Qian Song, Xianwen Yang, Yuduo Wei, Qi Hu, Libin Liu, and Ligang Zhang. 2022. "Experimental Investigation of the Phase Relations in the Fe-Zr-Y Ternary System" Materials 15, no. 2: 593. https://doi.org/10.3390/ma15020593

APA Style

Li, C., Song, Q., Yang, X., Wei, Y., Hu, Q., Liu, L., & Zhang, L. (2022). Experimental Investigation of the Phase Relations in the Fe-Zr-Y Ternary System. Materials, 15(2), 593. https://doi.org/10.3390/ma15020593

Note that from the first issue of 2016, this journal uses article numbers instead of page numbers. See further details here.

Article Metrics

Back to TopTop