Nanosized Sodium-Doped Lanthanum Manganites: Role of the Synthetic Route on their Physical Properties

In this paper we present the results of the synthesis and characterisation of nanocrystalline La1-xNaxMnO3+delta samples. Two synthetic routes were employed: polyacrylamide-based sol-gel and propellant synthesis. Pure, single phase materials were obtained with grain size around 35 nm for the sol-gel samples and around 55 nm for the propellant ones, which moreover present a more broaden grain size distribution. For both series a superparamagnetic behaviour was evidenced by means of magnetisation and EPR measurements with peculiar features ascribable to the different grain sizes and morphology. Preliminary magnetoresistivity measurements show enhanced low-field (< 1 T) magnetoresistance values which suggest an interesting applicative use of these manganites.Comment: 31 Pages 10 Figures to appear in Chem. Mate

Síntese e caracterização estrutural do niobato de potássio e estrôncio com estrutura tipo Tetragonal Tungstênio Bronze TTB Synthesis and structural characterization of strontium potassium niobate oxide with tetragonal tungstenium bronze TTB type structure

A fase nanoestruturada KSr2Nb5O15, foi sintetizada pelo método de mistura mecânica de óxidos por moagem de alta eficiência e por via química, utilizando o método dos precursores poliméricos, em forno tipo tubo sob atmosfera de O2 durante 10 h. A análise por difração de raios X dos pós calcinados a 1150 ºC foi realizada pelo método de Rietveld utilizando-se o software FullProf. A análise dos parâmetros estruturais obtidos via método de Rietveld mostrou um sistema tetragonal com estrutura tipo tetragonal tungstênio bronze. A partir das reflexões observadas, há apenas evidência da regra [(0kl) k = 2n], a qual é compatível com o grupo espacial centrossimétrico P4bm, o qual foi utilizado para o refinamento. O volume da célula unitária obtido na análise dos pós de KSr2Nb5O15 obtidos por síntese química e por moagem de alta eficiência foi 611,90 ų e 611,95 ų, respectivamente.<br>The nanostructured KSr2Nb5O15 phase was synthesized by both routes, the high efficiency milling and the polymeric precursor, in a furnace under O2 atmosphere during 10 h. The Rietveld X-ray diffraction analysis of the calcined powders at 1150 ºC was performed using the FullProf software. The XRD pattern analysis showed a tetragonal system with the tetragonal tungsten bronze structure. From the observed reflections, there is only evidence of the rule existence [(0kl) k = 2n], which is compatible with the centrosymmetric space group P4bm, which was used for the refinement. The unit cell volume obtained for the KSr2Nb5O15 powders prepared by chemical synthesis and by high efficiency milling were equal to 611,90 ų and 611,95 ų, respectively