Structural, Morphological, Differential Scanning Calorimetric and Thermogravimetric Studies of Ball Milled Fe Doped Nanoscale La 0.67 Sr 0.33 MnO 3 Manganite NIDHI ASTIK, 1 PRAFULLA K. JHA , 1,3 and ARUN PRATAP 2 1.—Department of Physics, Faculty of Science, The M. S. University of Baroda, Vadodara 390002, India. 2.—Department of Applied Physics, Faculty of Technology and Engineering, The M. S. University of Baroda, Vadodara 390001, India. 3.—e-mail: prafullaj@yahoo.com The ball milling route has been used to produce the La 0.67 Sr 0.33 Mn 0.85 Fe 0.15 O 3 (LSMFO) nanocrystalline sample from oxide precursors. The sample was characterized using x-ray diffraction (XRD), a scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDAX), differential scanning calorimetry (DSC) and thermogravimetric (TGA) measurements. The x-ray diffraction confirms the phase purity of sample and shows that the sample crystallizes in the rhombohedral perovskite structure with a R-3c space group. The scanning electron micrograph shows the presence of well-faceted crys- tallites of LSMFO. The EDAX spectrum demonstrates the molar ratio of dif- ferent elements of nanocrystalline LSMFO. Furthermore, the crystallite size using the Debye–Scherrer formula and William-Hall analysis has been found as 24 nm and 29 nm, respectively. Our results support the idea that a good quality nanocrystalline LSMFO sample can be obtained using the ball milling route. We also discuss the DSC and TGA curves and analyse the results in terms of phase transition, calcination temperature and activation barrier energies. Key words: Manganites, ball-milling, calcinations, XRD, SEM-EDAX, DSC, TGA INTRODUCTION There has been continuing interest in the study of doped rare-earth manganite perovskites with gen- eral formula Ln 1x A x MnO 3 , (where Ln = La, Nd, Sm… rare earth ions and A = Ba, Sr, Pb and Ca; divalent alkaline earth ions) due to their peculiar physical properties arising from the strong coupling between spin, charge, orbit and lattice degrees of freedom and observed colossal magnetoresistance (MR) effect in them. 1–9 These doped manganites exist in a verity of phases of perovskite structure and have their potential applications in transducer and sensor, catalysis, permanent magnets, high temperature superconducting, novel electronic materials and solid oxide fuel cells. 10–17 It is a widely recognized fact that the pairs of Mn 3+ and Mn 4+ ions play a major role in double exchange (DE) interaction for the ferromagnetic and metallic prop- erties in these manganese oxides. The DE effect arises due to the exchange of electrons from neigh- bouring Mn 3+ to Mn 4+ ions through oxygen when their core spins are parallel and hopping is not favoured for anti-parallel spins. 18 Furthermore, an additional mechanism, Jahn–Teller distortion (JT), has also been found responsible for the transport properties in these compounds. The JT effect causes further degeneracy of the e g orbital of the Mn 3+ in MnO 6 octahedral and results in electrical transport via hopping. 19–21 There are several methods, such as the solid state reaction, sol–gel and ball milling for the preparation of homogeneous samples of these materials required in various industrial appli- cations. 22–24 It is found that the substitution of (Received July 8, 2017; accepted November 22, 2017) Journal of ELECTRONIC MATERIALS https://doi.org/10.1007/s11664-017-5994-7 Ó 2017 The Minerals, Metals & Materials Society