Infraestructure and facilities

X-Ray Diffraction Platform

Brüker Nanostar (SAXS-Small Angle X-ray Scattering instrument)

SAXS (Small-Angle X-ray Scattering) is a reliable, economic and non-destructive method for analyzing nanostructured materials, yielding information on particle sizes and size distributions from 1 to 100 nm, shape and orientation distributions in liquid, powders and bulk samples. In Bruker Nanostar a brilliant X-ray source is combined with innovative multi-layer optics, which provides an intense, point-like incident beam upon the sample. Thanks to the 3-pinhole collimation, the background is extremely low, which is a must for the analysis of weakly scattering samples. The VÅNTEC-2000 is a large 2-D detector with true photon counting ability, featuring a maximum performance in angular resolution, low background and dynamic range. Such a large 2-dimensional detector is essential for SAXS measurements as it avoids any potential misinterpretation of data, eliminating the need for restrictive initial assumptions about the sample. In fact, the NANOSTAR analyzes pure sample properties, even for non-isotropic sample systems. Additionally, a real space image with µm SAXS resolution of the sample can be taken by performing Nanography. Samples can be solids (powder, ceramic, polymer, crystal) or liquid materials (polymers, colloidal particles in solution etc...).

BRUKER - D8 X-ray diffractometer

The D8 ADVANCE is an all-purpose X-ray analyser which can be configured for all powder diffraction applications, including phase identification, quantitative phase analysis, micro-structure and crystal structure analysis. The system can operate in both divergent and parallel beam geometries and is equipped with a LYNXEYE detector. The LYNXEYE is a 1-dimensional "compound silicon strip" detector for ultra-fast X-ray diffraction measurements. Implemented with the LYNXEYE, high quality diffraction data can be acquired with unprecedented speed, more than 150 times faster than a conventional point detector system. Temperature chambers are available for a broad range of temperatures (-190ºC-1200ºC) and under different atmospheres (Nitrogen, Helium, Oxygen, Air, Vacuum). Special accessories for air-sensitive samples as well as an electrochemical cell for in situ studies are also available.

Bruker D8 DISCOVER

The D8 DISCOVER is an all-purpose X-ray analyser which can be configured for a great of range diffraction applications: powder diffraction, including phase identification and quantitative phase analysis, micro-structure and crystal structure analysis, film analysis, residual stress and texture investigations. The system can operate in both divergent and parallel beam geometries and is equipped with a LYNXEYE XE detector. The LYNXEYE XE is the first energy dispersive 1-dimensional detector operating at room temperature for ultra fast X-ray diffraction measurements. It is developed on the basis of compound silicon strip technology and is specially optimized to meet the demands of X-ray diffraction in terms of highest count rate capabilities, best angular resolution (FWHM), and best energy solution. The LYNXEYE XE is the highest performing detector on the market in terms of both data quality and manufacturing quality, as manifested by high-speed data acquisition up to 450 times faster than a conventional point detector system. It is equipped with Vario1 monochromator system which removes unwanted characteristic radiation components such as Kβ, Kα2. This minimize the peak overlap especially in the higher angular region. Furthermore the peak-to-background ratio is increased due to background suppression.  Both effects significantly enhance the detection limits of minor phase amounts.

X-Ray Diffractometre XRD allows chemical and physical characterization through the identification of crystalline materials and their structural determination.  Structural and morphological changes of materials under temperature changes or electrochemical cycling can also be followed. Through XRD the following can be determined: unit cell parameters and atomic content for pure crystalline samples, phase identification, microstructure (crystallite size, shape and strains), phase transitions, reaction mechanisms. We can offer the study of solid materials through measurements under different temperatures and atmospheres as well as upon cycling in an electrochemical cell. SAXS Small angle neutron scattering (SAXS) is complementary to XRD by focusing on the smaller angles, before the first diffraction peaks appear, giving information on disordered or amorphous matter that may not give significant XRD signal, and in a general way on the microstructure of the matter (phase separation, porosity, nanoparticles, aggregates, polymer topology and organization etc...) in the range 0.3-100nm. Hence, the topology in the range 0.3-100nm of materials can be studied, in order to relate their microstructural features to their physic-chemical properties. We can offer the study of solid and liquid materials (either as pure materials or composites), liquid solutions as well as electrodes that have been cycled in electrochemical cell. Measures are done at room temperature and under vacuum (10-4 Torr).

Head of the Unit

Dr. Montse Casas - Cabanas
Dr. Montse Casas - Cabanas

Dr. Montse Casas-Cabanas completed her Ph.D. in Materials Science at Institut de Ciència de Materials de Barcelona (ICMAB) in 2006, where she worked on the positive electrode in nickel based batteries.  During a stay in Laboratoire Léon Bruillouin (LLB-CEA Saclay, France) in 2004 she developed in collaboration with Dr. Juan Rodríguez-Carvajal the FAULTS program for the refinement of XRD diffraction patterns of faulted materials. After her Ph.D. she joined the Laboratoire de Réactivité et Chimie des Solides (LRCS, Amiens, France) as a post-doctoral researcher where she was involved in the crystallochemical characterization of lithium-ion battery materials from powder diffraction. She also spent one year at Electron Microscopy for Materials Science (EMAT, Antwerp, Belgium) as a post-doctoral researcher where she applied transmission electron microscopy to the study of materials for energy storage and conversion. Before joining CIC Energigune she was Maître des Conferences at Laboratoire de Cristallographie et Sciences des Materiaux (CRISMAT, Caen, France) working on energy related materials.  Her research focuses on the impact of structure and microstructure in the electrochemical properties of energy storage materials and its study from diffraction techniques.

Publications

2017
Title:
EFFECT OF THE M3+ CATION SIZE ON THE STRUCTURAL AND HIGH TEMPERATURE PHASE TRANSITIONS IN SR2 MSBO6 (M = LN, Y) DOUBLE PEROVSKITES
Authors:
B. Orayech, A. Faik, J.M. Igartua
Journal:
[Polyhedron ]
DOI:
10.1016/j.poly.2016.09.066
2016
Title:
THE EFFECT OF PARTIAL SUBSTITUTION OF NI BY MG ON THE STRUCTURAL, MAGNETIC AND SPECTROSCOPIC PROPERTIES OF THE DOUBLE PEROVSKITE SR2NITEO6
Authors:
B. Orayech, L. Ortega-San-Martín, I. Urcelay-Olabarria, L. Lezama,?T. Rojo, María I. Arriortua and?J. M. Igartua
Journal:
[Dalton Transactions]
DOI:
10.1039/C6DT02473D
Title:
HIGH TEMPERATURE INDUCED PHASE TRANSITIONS IN SRCACOTEO6 AND SRCANITEO6 ORDERED DOUBLE PEROVSKITES
Authors:
A. Zaraq, B. Orayech, A. Faik, J.M. Igartua, A. Jouanneaux and A. El Bouari
Journal:
[Polyhedron ]
DOI:
10.1016/j.poly.2016.02.041
2015
Title:
SYNTHESIS, CRYSTAL STRUCTURE AND VIBRATIONAL SPECTROSCOPY STUDIES OF THE LACUNAR APATITE NAPB2CA2(PO4)3
Authors:
A. Chari , B. Orayech , A. Faik , J. M. Igartua , A. El Bouari
Journal:
[Journal of Materials and Environmental Science]
DOI:
Title:
SYNTHESIS AND ELECTRICAL PROPERTIES SOLID SOLUTION OF THE (1-X)BIO1.5- (X/4)NB2TE2O9 (X=0.1, 0.2) TYPE δ-BI2O3
Authors:
L. Loubbidi , A. Chagraoui , S. Villain , L. Bourja , B. Orayech , O. Ait Sidi Ahmed , A. Moussaoui , A. Tairi
Journal:
[Journal of Materials and Environmental Science]
DOI:
Title:
LOCAL MECHANICAL PROPERTIES OF GRAPHENE/POLYETHYLENE-BASED NANOCOMPOSITES BY DEPTH-SENSING INDENTATION
Authors:
Araceli Flores, Fernando Ania, Horacio J. Salavagione, Gary Ellis, Damien Saurel, Marián A. Gómez-Fatou
Journal:
[European Polymer Journal]
DOI:
10.1016/j.eurpolymj.2015.11.016

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Fees X-Ray Diffraction Platform

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