Magnetic, transport, and thermodynamic properties of CaMn 2 O 4 single crystals B. D. White, 1 J. A. Souza, 1, * C. Chiorescu, 2 J. J. Neumeier, 1, and J. L. Cohn 2 1 Department of Physics, Montana State University, P.O. Box 173840, Bozeman, Montana 59717-3840, USA 2 Department of Physics, University of Miami, Coral Gables, Florida 33124, USA Received 9 December 2008; revised manuscript received 12 February 2009; published 24 March 2009 Physical properties including magnetic susceptibility, room-temperature electrical resistivity, thermal con- ductivity, heat capacity, and thermal expansion are reported for high quality single-crystal samples of marokite CaMn 2 O 4 . We determined that CaMn 2 O 4 is highly electrically insulating and exhibits long-range antiferro- magnetic order below T N = 217.5 0.6 K with easy axis along a. Anisotropic thermal expansion, similar to that of crystallographically layered materials, is observed, suggesting that the crystal structure of CaMn 2 O 4 is also assembled from previously undescribed layers. An extensive thermodynamic study of the antiferromagnetic transition was undertaken resulting in a heat-capacity critical exponent = 0.082 0.007 and calculated pres- sure derivative dT N / dP = 5.154 0.174 K / GPa. DOI: 10.1103/PhysRevB.79.104427 PACS numbers: 75.47.Lx, 75.50.Ee, 71.70.Ej, 65.40.De I. INTRODUCTION Initial studies of CaMn 2 O 4 were published shortly after its discovery in 1963 in Morocco as a naturally occurring mineral. 1 It was subsequently named marokite for its country of origin and was found to crystallize in an orthorhombic structure with space group 2 Pbcm and exhibit antiferromag- netic AFMordering below 225 K. 3 But in the decades fol- lowing these preliminary investigations, further studies are completely absent in the literature until 2001, when CaMn 2 O 4 was studied as an impurity phase in the solid-state synthesis of manganese oxides exhibiting colossal magne- toresistance behavior. 4 CaMn 2 O 4 has since enjoyed some re- newed interest; however, recently published studies have been primarily limited to reporting on aspects of the mag- netic ordering 46 and crystal structure. 4,5,7 An extensive physical property characterization of CaMn 2 O 4 has yet to be conducted. Compounds with chemical formula AB 2 O 4 frequently crystallize in the cubic spinel structure with space group Fd3m or a tetragonally distorted spinel structure with space group I4 1 / amd. This is true of several manganese oxide compounds: NMn 2 O 4 with N =Ni, Cu, Mn, Zn, Cd, Mg, and Li. 8,9 The crystal structure of CaMn 2 O 4 is displayed in Fig. 1 as generated by JAVA STRUCTURE VIEWER. 10 It is primarily constructed from a complex network of MnO 6 octahedra. We can formulate a convenient description of this network by considering zigzag layers of edge-sharing octahedra running parallel to b, which are coupled along c by vertex sharing of apical oxygen sites. All MnO 6 octahedra are oriented with one of two tilted orientations with respect to the c axis and, while all octahedra display the same tilt orientation within each layer, successive zigzag layers alternate between the two. Tunnels along a between the zigzag layers are occupied by Ca 2+ ions. In stoichiometric CaMn 2 O 4 , all manganese ions are nominally high-spin Mn 3+ 3d 4 , t 2g 3 e g 1 . This elec- tronic configuration is well known to result in highly Jahn- Teller JTdistorted MnO 6 octahedra. Neutron-diffraction studies observe 26% elongation of the axial Mn-O bond dis- tances relative to equatorial in the octahedra. 4 The magnitude of this distortion certainly excludes the possibility of a cubic spinel structure for CaMn 2 O 4 but does not directly prevent the stabilization of a tetragonally distorted spinel structure. However, the large Ca 2+ ions do inhibit tetragonal symmetry. The A site in the spinel structure is located in a position which forms AO 4 tetrahedra. Comparison of the ionic radii of all divalent ions occupying a tetrahedral site reveals that Ca 2+ has the largest ionic radius of any with only Pb 2+ and Hg 2+ being slightly smaller. 11 Most other divalent ions in this situation those generally occupying the A site of compounds which do crystallize in the spinel structurehave ionic radii 50%–70% as large as Ca 2+ 1.00 Å. 11 The structure of CaMn 2 O 4 is stabilized when Ca 2+ incorporates itself into eightfold coordination with CaO 8 polyhedra instead of CaO 4 tetrahedra. 4,5 Many cubic spinel compounds exhibit a struc- tural phase transition under pressure to one of three related orthorhombic structures—those of CaMn 2 O 4 Pbcm, CaFe 2 O 4 Pnma, and CaTi 2 O 4 Cmcm. 8 This observation FIG. 1. Color onlineCrystal structure of CaMn 2 O 4 viewed roughly along a perspective has small c-axis component to visually clarify details of the three-dimensional 3Dstructure. MnO 6 octa- hedra are explicitly displayed within a single unit cell revealing a complex network with large Ca 2+ ions occupying tunnels along a between zigzag layers built along b. PHYSICAL REVIEW B 79, 104427 2009 1098-0121/2009/7910/1044279©2009 The American Physical Society 104427-1