Magnetic ordering effects in the Raman spectra of La 1 x Mn 1 x O 3 E. Granado, A. Garcı ´ a, J. A. Sanjurjo, C. Rettori, and I. Torriani Instituto de Fı ´sica ‘‘Gleb Wataghin,’’ UNICAMP, 13083-970, Campinas-SP, Brazil F. Prado, R. D. Sa ´ nchez, and A. Caneiro Centro Ato ´mico Bariloche and Instituto Balseiro, Comisio ´n Nacional de Energı ´a Ato ´mica and Universidad Nacional de Cuyo, RA-8400 San Carlos de Bariloche, Argentina S. B. Oseroff San Diego State University, San Diego, California 92182 Received 21 January 1999; revised manuscript received 2 June 1999 Temperature-dependent Raman spectra of polycrystalline La 1-x Mn 1-x O 3 samples, referred to as LaMnO 3+ for convenience, were correlated to their structural and magnetic properties for different . For 0.05, a softening of the 610 cm -1 Raman mode is observed below the magnetic ordering temperature. This softening is reduced as increases from 0.00 to 0.05. This behavior is not associated with lattice anomalies, and is interpreted in terms of a spin-phonon coupling caused by a phonon modulation of the superexchange integral. A quantitative analysis of this effect is presented. S0163-18299910737-9 In recent years, much effort has been devoted to under- standing the physics involved in the transport and magnetic phenomena of perovskite manganites. It was claimed that the early double-exchange DEtheory 1 cannot explain quantitatively the large conductivity drop near the ferromagnetic-paramagnetic FM-PMtransitions for doped compounds. 2 The presence of lattice polarons, possibly en- hanced by the strong Jahn-Teller character of the Mn 3 + ion, has been invoked to explain the large change in electron kinetic energy at T T C , 2 as well as other anomalous physi- cal properties of these materials. 3–5 Such polarons are ex- pected to be present when h -1 , where h is the electron transfer time and is the frequency of an optical-mode lattice vibration associated with a dynamic Jahn-Teller distortion, 6 i.e., a stretching mode. Therefore, lattice vibra- tions possibly play an important role in the conduction mechanism of this class of materials. Although the parent compound LaMnO 3 is an antiferromagnetic AFMinsulator, the study of the lattice and magnetic properties of this mate- rial may be taken as a starting point to a consistent under- standing of the more complex physical properties of the doped compounds. Perovskites with an orthorhombic Pnma space group present 24 Raman active modes (7 A g +5 B 1 g +7 B 2 g +5 B 3 g ). Lattice dynamical calculations and assignment of the Raman modes of LaMnO 3 were done previously by Iliev et al. 7 In a recent work, we reported a softening of the 604 cm -1 stretching mode below T N for the orthorhombic LaMnO 3.0 , 8 also observed by others. 9 This effect was asso- ciated with spin-phonon interactions, 9 and exchange striction effects. 8 Nevertheless, a detailed study that explains the soft- ening of the 604 cm -1 stretching mode in LaMnO 3 is still missing. In this work, we present Raman and x-ray studies of the LaMnO 3 + controlled oxygen content series ( 0.07). We conclude that the observed anomalous shifts for the 610 cm -1 mode in the samples with 0.05 are due to a phonon modulation of the xz -plane superexchange integral and not to the lattice anomalies observed below the magnetic transitions. From a first-neighbors contribution, we obtain the value of the second derivative of the xz -plane superex- change integral with respect to the stretching oxygen dis- placements in the Mn-O( xz ) direction. In this paper, for simplicity, the nomenclature LaMnO 3 + is used. However, we should mention that the O 2 - ions can- not be accomodated interstitially in the lattice. Thus, from a crystallographic point of view, the correct formula for this series is La 1 -x Mn 1 -x O 3 with x /3. 10 General properties of cation-deficient samples with the La 1 -x Mn 1 -y O 3 formula have been systematically studied in the literature. 10–14 The LaMnO 3 + samples studied in this work were grown by different methods. Samples with =0.00, 0.03, 0.05, and 0.07 were prepared following the nitrate decomposition method using Mn and La 2 O 3 as starting materials. 15 The sample referred to as LaMnO 3 : Ar annealed was prepared by standard ceramic methods, heating stoichiometric mixtures of the corresponding oxides. 16 The structure and phase purity of the samples were checked by x-ray powder diffraction. Well resolved x-ray patterns were obtained with Cu K ra- diation of a Rigaku conventional source and a high- resolution diffractometer with low-temperature attachment. Lattice parameters were obtained using a Rietveld refinement program. 17 Magnetization dc/acmeasurements have been taken in a Quantum Design PPMS magnetometer. Details of the Raman experimental setup are given elsewhere. 8 Except for the x-ray experiments, all the measurements as a function of T were done with increasing temperature. A summary of the structural and magnetic properties of the studied samples is given in Table I. The Ar annealed sample and those with =0.00 and 0.03 are mainly AFM with a FM component that increases with . For simplicity, we will refer to all these samples as AFM. The sample with =0.07 is FM. Finally, the sample with =0.05 presents a complex magnetic behavior that can be ascribed to frustrated FM or mixed FM/AFM phases. 15 All the samples studied in this work present orthorhombic Pnma crystal structure be- tween 15 and 300 K. PHYSICAL REVIEW B 1 NOVEMBER 1999-I VOLUME 60, NUMBER 17 PRB 60 0163-1829/99/6017/118794/$15.00 11 879 ©1999 The American Physical Society