Structural Determination, Unstable Antiferromagnetism and Transport Properties of Fe-Kagome Y0.5Fe3Sn3 Single Crystals

Yang Liu; Meng Lyu; Junyan Liu; Shen Zhang; Jinying Yang; Zhiwei Du; Binbin Wang; Hongxiang Wei; Enke Liu

doi:10.1088/0256-307X/40/4/047102

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Structural Determination, Unstable Antiferromagnetism and Transport Properties of Fe-Kagome Y_0.5Fe₃Sn₃ Single Crystals

1.
School of Rare Earths, University of Science and Technology of China, Hefei 230026, China
2.
Ganjiang Innovation Academy, Chinese Academy of Sciences, Ganzhou 341000, China
3.
Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, Beijing 100190, China
4.
School of Physical Sciences, University of Chinese Academy of Sciences, Beijing 100049, China
5.
Guobiao (Beijing) Testing & Certification Co., Ltd., Beijing 100088, China

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Corresponding author:
Enke Liu, E-mail: ekliu@iphy.ac.cn

Received Date: February 09, 2023

Published Date: March 01, 2023

Abstract

Abstract

Kagome materials have been studied intensively in condensed matter physics. With rich properties, various Kagome materials emerge during this process. Here, we grew single crystals of Y_0.5Fe₃Sn₃ and confirmed an YCo₆Ge₆-type Kagome-lattice structure by detailed crystal structure characterizations. This compound bears an antiferromagnetic ordering at T_N = 551 K, and shows a weak ferromagnetism at low temperatures, where an anomalous Hall effect was observed, suggesting the non-zero Berry curvature. With the unstable antiferromagnetic ground state, our systematic investigations make Y_0.5Fe₃Sn₃ a potential Kagome compound for Kagome or topological physics.

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Kagome materials, featuring a Kagome lattice consisting of geometric frustrated corner-sharing triangles,^[1] have attracted widespread interests due to the peculiar characteristics such as Dirac point, flat band, and Van Hove singularities in the electronic bands. As of now, abundant Kagome materials have been discovered to exhibit intriguing properties. Co-based Kagome material Co₃Sn₂S₂ is confirmed as the first magnetic Weyl semimetal, behaving giant anomalous Hall effect, negative magnetoresistance effect and so on.^[2–5] Mn-based Kagome material Mn₃X (X = Ge, Sn) is a non-collinear antiferromagnet with Weyl fermions, which surprisingly exhibits large anomalous Hall effect and anomalous Nernst effect.^[6–9] The most popular material in condensed matter physics in the past two years is V-based Kagome material AV₃Sb₅ (A = K, Rs, Cs) because of the topological superconductivity,^[10–15] while newly reported Ru-based Kagome material YRu₃Si₂ is a type-II superconductor with strong electron correlations.^[16] Moreover, in strongly correlated systems, some Kagome materials with frustrated magnetism exhibit spin liquid behavior, such as Cu-based Kagome material ZnCu₃(OH)₆Cl₂^[17–19] and Hyperkagome material Na₄Ir₃O₈.^[20] In a word, Kagome materials provide a great platform to explore new quantum states and fascinating physical properties.

To better understand the mechanism of Kagome physics, the exploration of new Kagome materials is urgently needed. In this Letter, we focus on the large Kagome family of RT₆Sn₆ (R represents rare-earth elements, T transition metal elements), where the Mn-based RMn₆Sn₆ and V-based RV₆Sn₆ have been widely studied to display topological properties, such as the quantum-limit Chern phase,^[21] electronic correlation effects,^[22] Dirac cone, flat band, and saddle point.^[23–26] However, Fe-based RFe₆Sn₆ is rarely reported up to date. In this work, we have synthesized the single-crystalline YFe₆Sn₆ and investigated its physical properties. In the previous reports, the crystal structure of YFe₆Sn₆ is ambiguous. There are three different structures proposed, one is the Kagome-lattice YCo₆Ge₆-type (P6/mmm) structure,^[27] the others are Cmcm^[28] and HoFe₆Sn₆-type (Immm) structure.^[29] In addition, there is no detailed research of physical properties about single crystals of this compound. Therefore, whether YFe₆Sn₆ is another Kagome material and the related properties are well worth further study.

By careful characterizations of crystal structure using x-ray diffraction (XRD) and transmission electron microscopy (TEM), it is confirmed that our single crystal of YFe₆Sn₆ employs an YCo₆Ge₆-type structure with Fe-Kagome layers. The result of the VSM Oven measure shows that it is an antiferromagnet at T_N = 551 K, and magnetic susceptibility measurements reveal that it undergoes a spin-reorientation at low temperatures. More surprisingly, the apparent anomalous Hall effect below 50 K is observed, suggesting the probable topological electronic bands in this antiferromagnetic compound.

Sample Growth and Composition Analysis. Single crystals of YFe₆Sn₆ were grown with the high-temperature Sn self-flux method.^[30,31] The starting elements of high-purity Y (ingots, 99.9%), Fe (pieces, 99.99%), and Sn (pellets, 99.999%) were combined in a molar ratio of 1:6:10, then placed in an alumina crucible and sealed in a silica tube. Afterward, the mixture was heated to 1100 °C and stayed for 24 h, then slowly cooled down to 700 °C within one week. Finally, the quartz tube was centrifuged at 700 °C to separate the excess Sn flux to obtain YFe₆Sn₆ single crystals. After the centrifugation, the residual Sn exposed on the crystal surfaces was removed with diluted hydrochloric acid. As shown in the inset of Fig. 1(b), the obtained single crystal sample shows a typical hexagonal thin pillar.

Fig. Fig. 1. Structural information of Y_0.5Fe₃Sn₃ compounds. (a) Crystal structure of Y_0.5Fe₃Sn₃. The atoms arranged along the c axis have only an occupancy rate of 50% due to their close sites, so the atoms are set relatively transparent. (b) XRD pattern of Y_0.5Fe₃Sn₃ single crystal with (l00) reflections at room temperature. Inset shows a photo of single-crystalline Y_0.5Fe₃Sn₃ samples with (l00) crystal face on a millimeter grid. (c) TEM pattern of Y_0.5Fe₃Sn₃ single crystal with (00l) atomic arrangement at room temperature. Inset shows an image of the electron diffraction with crystal plane orientation. (d) Laue pattern of Y_0.5Fe₃Sn₃ single crystal with (00l) reflections at room temperature.

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The composition analysis was performed on a Hitachi S-4800 scanning electron microscope (SEM) with the energy dispersive x-ray spectroscopy (EDS). Several batches of crystals were selected to carry out EDS measurements, the results show Y : Fe : Sn ∼ 0.9:6:6.1, close to 1:6:6, demonstrating that the as-grown crystals employ the desired chemical composition.

Crystal Structure. First of all, it is apparent that YFe₆Sn₆ may adopt a hexagonal structure because of the typical hexagonal prism shape of the obtained crystals. Then, we performed single crystal XRD (D2 Phaser, Bruker) diffraction experiments on the exposed crystal planes of the samples and obtained the results as shown in Fig. 1(b). It can be found that the diffraction peak positions are close to the (l00) peak positions of the YCo₆Ge₆-type and the HfFe₆Ge₆-type structure by comparing the standard structure analysis. The YCo₆Ge₆-type and the HfFe₆Ge₆-type structure are both P6/mmm space group but there are some differences in the atomic arrangement of the two types. In fact, the YCo₆Ge₆-type structure is nested by two sets of HfFe₆Ge₆-type unit cells, one of which is translated by c/2 relative to the other HfFe₆Ge₆-type unit cell,^[32] as shown in Fig. 2. At the same time, since the atoms arranged along the c axis occupy the relatively near positions in the YCo₆Ge₆-type structure, these atomic positions only have an occupancy rate of 50%. Further, if the rare-earth atom layer is removed from the structure of Fig. 2(c), the HfFe₆Ge₆-type structure will turn to the CoSn-type structure, in which Sn atoms moves to the Fe atom layer along the c axis, as shown in Fig. 2(d). Afterwards, we performed transmission electron microscope (TEM) structure analysis on the single crystal sample. In Fig. 1(c), it is observed that the arrangement in the ab plane is a hexagonal lattice, which is consistent with the shape of the single crystal. Additionally, the exact crystal facet index is provided via the inset of the electron diffraction picture. In order to determine which kind of hexagonal structure the as-grown crystal is, we conducted further experiments. In Fig. 1(d), the Laue diffraction pattern of the (00l) plane is depicted, showing a six-fold rotational symmetry. The result is closer to the simulation of the YCo₆Ge₆-type structure. Therefore, we essentially deem that the structure of YFe₆Sn₆ single crystal is similar to the YCo₆Ge₆-type structure, as seen in Fig. 1(a), where a Kagome-lattice layer made of Fe atoms is present. In further detail, the stoichiometric ratio of elements in the unit cell of the YCo₆Ge₆-type structure is 0.5:3:3, so the chemical formula of the as-grown crystals should be expressed as Y_0.5Fe₃Sn₃.

Fig. Fig. 2. Crystal structure of YCo₆Ge₆-type Y_0.5Fe₃Sn₃: (a) showing all possible atomic positions, (b) and (c) showing two disordered structures, each occurring in 50% of cases, according to (a). If the rare-earth atom layer is removed from the structure of (c) and then the structure turns to CoSn-type structure (d).

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To further confirm the crystal structure of Y_0.5Fe₃Sn₃, the single crystal XRD refinement analysis was performed. The result demonstrates that our single crystal indeed employs the YCo₆Ge₆-type structure (P6/mmm space group). However, the careful analysis shows that it is slightly deviated from the primitive atomic occupancy of YCo₆Ge₆-type structure, where the Y atoms occupy the exact sites, and some Fe and Sn atoms are mixed from each other, but Fe atoms cannot occupy the positions of Sn atoms on the ab plane. Fe atoms may appear on the c-axis edge, that is, the arrangement of atoms on the c-axis edge is either Fe–Fe, or Sn–Sn, or Sn–Fe–Sn. The obtained refinement results of the sample given by single crystal XRD analysis are listed in Table 1.

Table 1. Crystal refinement of Y_0.5Fe₃Sn₃ single crystals.

Items	Parameters
Chemical formula	Y_0.50Fe_3.30Sn_2.93
Formula weight	576.60 g/mol
Crystal system	Hexagonal
Space group	P6/mmm
Unit cell dimensions	a = 5.3728(4) Å α = 90°
	b = 5.3728(4) Å β = 90°
	c = 4.4534(4) Å γ = 120°
Volume	111.333(19) Å³
Z	1
Density (calculated)	8.600 g/cm³

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Magnetic Properties. The magnetic and transport properties of Y_0.5Fe₃Sn₃ single crystals have not been reported before, so we have carried out experimental research on its relevant physical properties. The magnetic properties of the Y_0.5Fe₃Sn₃ single crystals were measured in a magnetic property measurement system (MPMS, Quantum Design) and the transport properties were measured in a physical property measurement system (PPMS, Quantum Design).

As shown in Fig. 3, the magnetic properties of Y_0.5Fe₃Sn₃ single crystal exhibits a strong anisotropy. Compared with B ∥ c, the magnetic moment is easily aligned when B ∥ ab. According to the measurements performed in the vibrating sample magnetometer oven (PPMS, Quantum Design), as seen in Fig. 3(a), we confirm that Y_0.5Fe₃Sn₃ is an antiferromagnet and its Neel temperature is 551 K. Figure 3(b) shows the temperature-dependent magnetic susceptibility of Y_0.5Fe₃Sn₃ with B ∥ c and B ∥ ab at B = 0.1 T, which clearly deviates from those expected for a simple antiferromagnet whose magnetic susceptibility decreases with decreasing temperature below T_N. They behave a rapid increase below 50 K, especially at B ∥ ab, signaling a probable spin-reorientation around this temperature region. Figure 3(c) presents the magnetization curves M (H) of Y_0.5Fe₃Sn₃ at T = 2 and 100 K. As seen in the plot, M (H) at T = 2 K is more easily to saturate compared to T = 100 K at B ∥ ab, and M (H) at B ∥ ab has a larger value of magnetization compared to M (H) at B ∥ c, again suggesting that the spin-reorientation results in the weak ferromagnetism in this compound. Most likely, the under-stoichiometry in the Y element is what causes these behaviors.^[33] For rare-earth intermetallic compounds, the rare-earth element R frequently has a significant impact on the sublattice magnetic anisotropy of the magnetic components. The under-stoichiometry in the Y element, known from the results of EDS, may yield small regions where basal plane and axial anisotropies compete. These regions interact with the magnetic exchange interaction of Fe atom layers to form magnetically frustrated regions. While in the frustrated regions, magnetic moments point between the basal plane and the c-axis, and this spin-orientation rearrangement results in the formation of small ferromagnetic component.^[34]

Fig. Fig. 3. Magnetic properties of Y_0.5Fe₃Sn₃ compounds. (a) VSM oven-measurement results indicating that T_N of the Y_0.5Fe₃Sn₃ compound is 551 K. (b) Temperature-dependent magnetic susceptibility of the Y_0.5Fe₃Sn₃ compound. (c) Field-dependent magnetization curves for the Y_0.5Fe₃Sn₃ compound at T = 2 and 100 K.

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Furthermore, the first-principles calculations were used to obtain the stable antiferromagnetic structure for Y_0.5Fe₃Sn₃, simulating the magnetic moments of Fe atoms arranged along out-of-plane (i.e., c axis) and in-plane (i.e., ab plane) directions, respectively, as shown in Figs. 4(a) and 4(b). It is worth noticing that the information of single crystal obtained by XRD refinement for Y_0.5Fe₃Sn₃ reveals the disordered atoms occupation and the closest arrangement of Sn atoms, and then the HfFe₆Ge₆-type structure was used for the first-principles calculations. The results of the calculations indicate that the magnetic moments of Fe atoms are energetically preferable to lay along in-plane directions. Figures 4(c) and 4(d) show the band structure and Fermi surface of the magnetic ground state. The parabolic band near the Fermi level appears at Γ point along high symmetry path K–Γ–M, while the band along Γ–A direction goes through the Fermi level, indicating two hole pockets and one electron pocket around Γ point along K–Γ–M directions and only a small electron pocket around Γ point along Γ–A direction, which are in agreement with the spherical Fermi surface in Fig. 4(d).

Fig. Fig. 4. (a) and (b) Two kinds of simulative antiferromagnetic structures of Y_0.5Fe₃Sn₃ compound using the HfFe₆Ge₆-type structure. (c) Energy bands along high-symmetry paths and (d) Fermi surface of Y_0.5Fe₃Sn₃ compound with moments laying in plane.

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Transport Properties. Consistent with the magnetic properties, the electric transport also exhibits clear anisotropy as shown in Fig. 5. Figure 5(a) displays the temperature-dependent electric resistivity curves ρ (T) of Y_0.5Fe₃Sn₃ with I ∥ ab and I ∥ c, which behaves a metallic electronic transport, that is, the longitudinal resistivity decreases with decreasing temperature in the entire temperature range from 300 to 2 K and the residual resistivity appears below about 50 K. Relative to the quasi-linear behavior of ρ_ab, ρ_c exhibits a strong curvature above 50 K, which may be caused by crystal electrical field interaction. Figures 5(b) and 5(c) present the anisotropic magnetoresistance (MR) of Y_0.5Fe₃Sn₃ with B ∥ c and B ∥ ab. It is observed that the MRs of both directions are relatively small, not more than 5%. The MR in ab plane is one order of magnitude larger than the out-of-plane MR. In addition, we note that both directions behave negative MR below 100 K, suggesting the possible ferromagnetic component in this compound, which is in agreement with the above discussion.

Fig. Fig. 5. Longitudinal transport properties of Y_0.5Fe₃Sn₃ compounds. (a) Temperature-dependent electric resistivity with I ∥ ab and I ∥ c. The inset cartoon shows the basic configuration of ab plane and c axis for the hexagonal sample. (b) Field-dependent magnetoresistance with B∥ c and I ∥ ab. (c) Field-dependent magnetoresistance with B ∥ ab and I ∥ c.

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Figure 6 shows the Hall effect of Y_0.5Fe₃Sn₃ with B ∥ c and B ∥ ab. In Figs. 6(a) and 6(b), it is seen that the Hall resistivity of both directions displays a linear behavior above 100 K, indicating that the single hole carriers dominate the transport properties. However, as temperature goes down below 100 K, the Hall effect bifurcates. The Hall resistivity ρ_yx and Hall conductivity σ_xy at B ∥ c show a typical multi-carrier behavior, which can be fitted by the two-carrier model:^[35]

$σ_{x y} (B) = \frac{n_{h} e μ_{h}^{2} B}{1 + μ_{h}^{2} B^{2}} - \frac{n_{e} e μ_{e}^{2} B}{1 + μ_{e}^{2} B^{2}} .$

(1)

As shown in the inset of Fig. 6(b), σ_xy measured at 2 K can be well fitted by Eq. (1), the carrier concentrations are estimated to be n_e = 4.9 × 10²² cm⁻³, n_h = 2.2 × 10²³ cm⁻³, and the carrier mobility μ_e = 43.7 cm²⋅V⁻¹⋅s⁻¹, μ_h = 20.8 cm²⋅V⁻¹⋅s⁻¹ at 2 K.

Fig. Fig. 6. Transverse transport properties of Y_0.5Fe₃Sn₃. (a) and (b) Field-dependent Hall resistivity and Hall conductivity with B ∥ c, I ∥ ab. Inset shows Hall resistivity and their fitting curves at 2 K by the two-carrier model and 100 K by the single-carrier model. (c) and (d) Field-dependent Hall resistivity Hall conductivity with B ∥ ab, I ∥ c. (e) The comparison of the Hall resistivity and the magnetization curve at T = 2 K in ab plane. Inset shows that the measured ρ_yx(B) at 2 K is decomposed into a normal and an anomalous Hall part. (f) Temperature-dependent in-plane AHC and AHA.

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Noticeably, at B ∥ ab, the Hall resistivity and Hall conductivity show a similar behavior of tending to saturation, seen in Figs. 6(c) and 6(d), apparently deviating from the multi-carrier feature. In consideration of the weak ferromagnetism in this compound as mentioned above, it is easy to conclude that the on-going saturated Hall resistivity is anomalous Hall effect. Figure 6(e) displays the comparison of the Hall resistivity and the magnetization curve at T = 2 K. Empirically, the Hall resistivity can be separated into the normal Hall part (

$ρ_{y x}^{N} = R_{0} B$ , R₀ is the ordinary Hall coefficient) and the magnetization related anomalous Hall part (

$ρ_{y x}^{A} = 4 π R_{s} M$ , R_s is the anomalous Hall coefficient and M is the saturation magnetization):

$ρ_{y x} = R_{0} B + 4 π R_{s} M .$

(2)

Thus, the value of R₀ obtained is 2.37 × 10⁻⁹Ω⋅m⋅T⁻¹ and further calculations show that the carrier concentration n_e is 2.63 × 10²¹ cm⁻³ and the carrier mobility μ_e is 21.0 cm²⋅V⁻¹⋅s⁻¹ at this time. The carrier concentration is two orders of magnitude smaller than that of the in-plane case, which is caused by the different bands in different directions. As mentioned above, in Figs. 4(c) and 4(d), there is only a small electron pocket on the Γ–A path but two hole pockets and an electron pocket on the K–Γ–M paths. The band structure is in agreement with the transport properties of Y_0.5Fe₃Sn₃, that is, it exhibits a single-carrier behavior and the lower carrier concentration for the out-of-plane case while a two-carrier behavior and the higher carrier concentration for the in-plane case. The inset plot of Fig. 6(e) shows that the Hall resistivity can be well separated by Eq. (2) at T = 2 K, which further consolidates the existence of the anomalous Hall effect in this compound. Furthermore, the anomalous Hall conductivity (AHC) and the anomalous Hall angle (AHA) can be calculated using the following equations:

$AHC = \frac{ρ_{y x}^{A}}{{(ρ_{y x}^{A})}^{2} + ρ_{x x} {(B = 0)}^{2}},$

(3)

$AHA = \frac{ρ_{y x}^{A}}{ρ_{x x} (B = 0)} .$

(4)

Here,

$ρ_{y x}^{A}$ is estimated from the high field linear part of

$ρ_{y x}^{A}$ , as shown in the inset of Fig. 6(e).

Figure 6(f) shows the AHC and AHA of Y_0.5Fe₃Sn₃, which behave the same trend of increase with decreasing temperature, and attain a saturation value of about 100 Ω⁻¹⋅cm⁻¹ and 1.1% below 10 K. Although the AHC and AHA of Y_0.5Fe₃Sn₃ are small, given that this compound is an antiferromagnet, such an apparent anomalous Hall effect is very intriguing. As we know, Mn₃Sn and Mn₃Ge^[6,7] are also constructed of a Kagome lattice, and show large anomalous Hall effect because of the nonzero Berry curvature from the nontrivial topological bands. A similar case may exist in Y_0.5Fe₃Sn₃. Therefore, to better understand the exotic transport properties of Y_0.5Fe₃Sn₃, the electronic energy bands are worthy of investigation in further study.

In summary, we have grown single crystals of Y_0.5Fe₃Sn₃ compound and performed the detailed structure characterization and physical property investigation. We confirm that this compound adopts an YCo₆Ge₆-type structure with Kagome lattice of Fe-layers. Y_0.5Fe₃Sn₃ compound is an antiferromagnet with high Neel temperature of 551 K, but there appears a weak ferromagnetism resulted from the spin-reorientation at low temperatures. The intriguing anomalous Hall effect is observed, suggesting the nonzero Berry curvature in this compound. Our study reveals that Y_0.5Fe₃Sn₃ is a new Kagome material, which provides a platform to study Kagome physics, topological physics, or correlation physics, and rare-earth magnetism by substituting Y to other magnetic rare-earth elements in future.

Acknowledgments.: This work was supported by the National Key R&D Program of China (Grant Nos. 2022YFA1403400, 2022YFA1403800, and 2019YFA0704900), the Fundamental Science Center of the National Natural Science Foundation of China (Grant No. 52088101), the Beijing Natural Science Foundation (Grant No. Z190009), the National Natural Science Foundation of China (Grant Nos. 11974394, 12174426, and 51271038), the Strategic Priority Research Program (B) of the Chinese Academy of Sciences (CAS) (Grant No. XDB33000000), the Key Research Program of CAS (Grant No. ZDRW-CN-2021-3), and the Scientific Instrument Developing Project of CAS (Grant No. ZDKYYQ20210003).

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Structural Determination, Unstable Antiferromagnetism and Transport Properties of Fe-Kagome Y_0.5Fe₃Sn₃ Single Crystals