Development of new characterization techniques: design and commissioning of a cell for simultaneous XRD and conductivity in-situ measurements

F. NAPOLITANO; A. SOLDATI; J. GECK; L. GIEBELER; A. FERNÁNDEZ ZUVICH; A. CANEIRO; A. SERQUIS; L. MOGNI

Mar del Plata

Congreso; X Reunión Anual de la Asociación Argentina de Cristalografía; 2014

Asociación Argentina de Crsitalografía

The design and development ofnew experimental techniques has been mostly driven by the need to gain a deeperinsight into the material?s properties, which could be used for fundamental orapplied research. Recent advances on materials characterization techniques haveprovided new platforms that enable the in-situstudy of crystallographic, mechanical, electronic, and electrochemicalproperties under a wide range of environmental conditions, not only forfundamental research but also in order to recreate a more realistic environmentin the case of applied research [1], [2], [3].In this context, thedevelopment of a device that enable the characterization of several propertiessimultaneously under controlled atmospheres in a wide range of temperaturesrepresents an advantage over the traditional independent measurements sincethose properties could be strongly correlated. As an example, in the SolidOxide Fuel Cells (SOFC) framework, the electrode materials have to present goodelectronic and ionic transport properties and also a good electrochemicalresponse to certain electrocatalytic reactions, being all these propertiesstrongly dependent of their crystallographic and electronic structures [4].In this work we present thedesign and implementation of a new high temperature cell that allows to, in afirst step, perform X-ray diffraction (XRD) and electrical conductivitymeasurements simultaneously between room temperature and 900 °C in an oxidizing,inert or vacuum atmospheres. Its design was conceived with several constrains:-         It should be easily adapted to a working Anton PaarHTK 1200 high temperature chamber.-         It should be portable in order to be carried tosynchrotron beamlines.-         It should be versatile, since several experimentaltechniques must be used without changes in the cell configuration: in-house orsynchrotron XRD, X-ray absorption spectroscopy (XANES/EXAFS), electricalconductivity, and electrochemical impedance spectroscopy.The first tests on this cellhave been performed on an in-house Panalytical Empyrean diffractometer withPixcel 3D detector, running simultaneous XRD and conductivity measurements.This work is funded byCONICET, CNEA and BMBF-MinCyT AL1013 project.  [1] M. Liu, M.E. Lynch, K.Blinn, F.M. Alamgir, Y.-M. Choi, Materials Today, 14(11) (2011) 534?546.[2] P.R. Shearing, R.S. Bradley,J. Gelb, S.N. Lee, A. Atkinson, P.J. Withers, N.P. Brandon, Electrochemical andSolid State Letters, 14(10) (2011) B117?B120.[3] S. Wolf, N.A. Cañas, K.A.Friedrich, Fuel Cells, 13(3) (2013) 404?409.[4] M. Imada, A. Fujimori, Y.Tokura, Reviews of Modern Physics, 70(4) (1998) 1039?1263.