DEVELOPMENT OF NEW CHARACTERIZATION TECHNIQUES: DESIGN AND COMMISSIONING OF A CELL FOR SIMULTANEOUS XRD AND CONDUCTIVITY IN-SITU MEASUREMENTS.

NAPOLITANO, FEDERICO; SOLDATI, ANALIA L.; GECK, JOCHEN; GIEBELER, LARS; FERNANDEZ ZUVICH, AFRA; SERQUIS, ADRIANA C.; CANEIRO, ALBERTO; MOGNI, LILIANA V.

Mar del Plata

Conferencia; AACr 2014; 2014

Asociación Argentina de Cristalografía

The design and development of new experimental techniques has been mostly driven by the need to gain a deeper insight into the material?s properties, which could be used for fundamental or applied research. Recent advances on materials characterization techniques have provided new platforms that enable the in-situ study of crystallographic, mechanical, electronic, and electrochemical properties under a wide range of environmental conditions, not only for fundamental research but also in order to recreate a more realistic environment in the case of applied research [1], [2], [3]. In this context, the development of a device that enable the characterization of several properties simultaneously under controlled atmospheres in a wide range of temperatures represents an advantage over the traditional independent measurements since those properties could be strongly correlated. As an example, in the Solid Oxide Fuel Cells (SOFC) framework, the electrode materials have to present good electronic and ionic transport properties and also a good electrochemical response to certain electrocatalytic reactions, being all these properties strongly dependent of their crystallographic and electronic structures [4]. In this work we present the design and implementation of a new high temperature cell that allows to, in a first step, perform X-ray diffraction (XRD) and electrical conductivity measurements 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 Paar HTK 1200 high temperature chamber. -        It should be portable in order to be carried to synchrotron beamlines. -        It should be versatile, in the way that several experimental techniques can be used without changes in the cell configuration: in-house or synchrotron XRD, X-ray absorption spectroscopy (XANES/EXAFS), electrical conductivity, and electrochemical impedance spectroscopy. The first tests on this cell have been performed on an in-house Panalytical Empyrean diffractometer with Pixcel 3D detector, running simultaneous XRD and conductivity measurements