Development of a new in-operando characterization instrumentation: Design and Commissioning of an Electrochemical cell for XRD/XAS coupled to Electrical/Electrochemical simultaneous measurements

F. NAPOLITANO; A. SOLDATI; A SERQUIS; J. BASBÚS; L. MOGNI

Campinas

Simposio; 27th RAU Annual Users Meeting; 2017

LNLS/CNPEM

Development of breakthrough technological devices is nowadays a highly complex task and requires an interdisciplinary teamwork. This challenge sometimes push toward the development of new ways to study the materials in order to acquire a comprehensive understanding of the involved processes; fundamental knowledge that allow the tailoring and optimization of the materials properties with the objective of obtain a commercially available technological device. 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].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.In this work we present the current state of an ongoing Long Term Proposal carried out at D10B-XPD and D08B-XAFS2 beamlines involving the design and implementation of a new high temperature cell that allows performing X-ray diffraction (XRD) or X-ray Absorption Spectroscopy (XAS) simultaneously with electrical conductivity measurements on dense samples or electrochemical characterization on porous electrodes. Its design was conceived with several constrains:- It should be versatile, several experimental techniques must 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.- It should be easily adapted to several high temperature chambers existing at LNLS and at CAB (Anton Paar HTK1200 and XRK900, Canario furnace). - It should be portable in order to be carried to synchrotron beamlines.We also present the measurements taken during the commissioning tests performed at XPD and XAFS2 beamlines (proposals #20150099 and #20170429, respectively) studying the correlation of the electronic properties of promising SOFC electrolyte materials with theirs crystallographic structure and XANES spectra evolution.