RAPID COMMUNICATIONS PHYSICAL REVIEW B 89, 020402(R) (2014) Hidden magnetic order in Sr 2 VO 4 clarified with μ + SR Jun Sugiyama, 1 , * Hiroshi Nozaki, 1 Izumi Umegaki, 1 Wataru Higemoto, 2 Eduardo J. Ansaldo, 3 Jess H. Brewer, 3, 4 Hiroya Sakurai, 5 Ting-Hui Kao, 5, 6 Hung-Duen Yang, 6 and Martin M˚ ansson 7, 8 1 Toyota Central Research and Development Laboratories Incorporated, Nagakute, Aichi 480-1192, Japan 2 Advanced Science Research Center, Japan Atomic Energy Agency, Tokai, Ibaraki 319-1195, Japan 3 TRIUMF, 4004 Wesbrook Mall, Vancouver, British Columbia, Canada V6T 2A3 4 Department of Physics and Astronomy, University of British Columbia, Vancouver, British Columbia, Canada V6T 1Z1 5 National Institute for Materials Science (NIMS), 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan 6 Department of Physics, National Sun Yat-Sen University, Kaohsiung 804, Taiwan 7 Laboratory for Quantum Magnetism (LQM), ´ Ecole Polytechnique F´ ed´ erale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland 8 Laboratory for Neutron Scattering, Paul Scherrer Institut, CH-5232 Villigen PSI, Switzerland (Received 17 September 2013; revised manuscript received 20 December 2013; published 6 January 2014) In order to elucidate the magnetic ground state of Sr 2 VO 4 , we have measured muon spin rotation and relaxation (μ + SR) spectra of a powder sample in the temperature range between 1.8 and 140 K. As a result, we have clarified that the transition at 105 K is not magnetic but structural and/or electric in origin and found the appearance of static antiferromagnetic (AF) order below 8 K. Moreover, the distribution of the internal AF field was found to be very broad, even at the lowest temperature measured. These results are consistent with the formation of an orbital-stripe order with collinear AF order for the magnetic ground state of Sr 2 VO 4 . DOI: 10.1103/PhysRevB.89.020402 PACS number(s): 75.25.Dk, 75.50.Ee, 75.70.Tj, 76.75.+i Tetragonal Sr 2 VO 4 with a K 2 NiF 4 -type structure has been considered as an analog of a parent compound of the first superconducting cuprate, i.e., La 2 CuO 4 , since the electron configuration of the V 4+ ion is t 1 2g with S = 1/2 in a tetragonal crystal field of a VO 6 octahedron [17]. Although susceptibility (χ m ) measurements clearly show a magnetic anomaly at 105 K (=T c )[6], a past neutron diffraction study reported the absence of magnetic peaks even at 5 K [2]. Since x-ray diffraction studies revealed a sudden enhancement of the c/a ratio below T c [6], it was proposed that an orbital-ordering transition occurs at T c . In fact, first principles calculations predicted an antiferromagnetic (AF) and orbital-ordered state with a nontrivial and large unit cell structure in the ground state, because of the coexistence and competition of ferromagnetic and AF exchange interactions [8,9]. Recently, a more exciting possibility was proposed, namely, that a hidden magnetic order is induced by spin-orbit coupling for a t 1 2g electron system [10]. Such work also predicted an unconventional magnetic octupolar ordering at low T for Sr 2 VO 4 . Furthermore, alternating spin-orbital order in the ab plane was proposed by considering the effects of spin-orbit coupling, crystal field, and superexchange on the energy levels of the V 4+ ions [11]. Despite the above attractive predictions, there are few reports on Sr 2 VO 4 utilizing microscopic magnetic techniques [12]. Macroscopic magnetic measurements such as χ m and neutron scattering usually give us significant insight into the ground state of magnetically ordered solids. However, such techniques are sometimes not suitable, particularly for the materials exhibiting order with a broad field distribution, i.e., when short-range order, random, or nearly random order appears in a material, due to the absence of periodic structure and/or the presence of rapid fluctuations. In contrast, the muon spin rotation and relaxation (μ + SR) technique is very sensitive * e0589@mosk.tytlabs.co.jp to local magnetic environments with a different time window compared to neutron scattering; thus μ + SR has provided crucial information on the magnetic ground state of materials [13,14]. We have therefore performed a μ + SR experiment on Sr 2 VO 4 and found the appearance of magnetic order not below T c but below 8 K. A powder sample of Sr 2 VO 4 was prepared from a precur- sor orthorhombic β -Sr 2 VO 4 [15], which was made from a stoichiometric mixture of SrO, V 2 O 3 , and V 2 O 5 by a solid state reaction at 1400 C in an Ar gas flow for 12 h. SrO was obtained by thermal decomposition of SrCO 3 at 1100 C for 12 h under vacuum, and V 2 O 3 was prepared from V 2 O 5 by reduction in an H 2 gas flow at 600 C for 4 h, and then at 800 C for 2 h. The obtained precursor was sealed in an Au capsule and then heated at 1300 C under 4 GPa. Powder x-ray diffraction (XRD) analyses revealed that the obtained sample was almost single phase of a K 2 NiF 4 - type structure with I 4/mmm space group [2]. Sr 3 V 2 O 8 was present in the sample at a level below 2%. This suggests that the average valence of the V ion in the whole sample is above 4+, implying the absence of oxygen deficiencies in Sr 2 VO 4 . χ m (=M/H , where M is magnetization) was measured below 400 K under a H 10 kOe field with a superconducting quantum interference device (SQUID) magnetometer. (See Fig. 1.) A Curie-Weiss fit in the T range between 110 and 320 K provided the T -independent term [χ 0 = 0.000 07(2) emu/mol], Weiss T [ CW =−28(4) K], and effective magnetic moment [μ eff = 1.36(2)μ B ]. These values are consistent with the literature [15]. The μ + SR time spectra were measured at TRIUMF in Canada in the T range between 1.8 and 140 K. The experimental techniques are described in more detail elsewhere [13]. Figures 2(a) and 2(b) show the zero field (ZF) and longitudinal field (LF) μ + SR spectra at 1.8 K. Here LF means the field is parallel to the initial muon spin polarization ( S μ ). The ZF spectrum exhibits rapid damping with a first minimum at t 0.25 μs, indicating the presence of a broad 1098-0121/2014/89(2)/020402(4) 020402-1 ©2014 American Physical Society