NAME X-ray Diffraction Platform

DESCRIPTION

CIC energiGUNE's X-ray diffraction platform offers a comprehensive service of X-ray diffraction and small angle scattering for the structural, micro-structural and morphological study of materials. It includes two powder diffractometers and a small angle scattering apparatus, together with temperature chambers, robot sample changers and an in-situ electrochemical cell of our own design. Structural analysis of materials can then be performed varying parameters such as atmosphere, temperature and oxidation state. The platform offers service of measurements as well as analysis of the results and is open to internal as well as external users.

FIELDS OF APPLICATION

Design and development of materials

Manufacturing processes

MOST OUTSTANDING EQUIPMENT AND COMPONENTS

  • Electrochemical cell for in-situ and operando PXRD and SAXS measurements

    Electrochemical cell, designed at CIC energiGUNE, that allow observing the changes in the Powder X-ray diffraction (PXRD) or Small Angle X-ray Scattering (SAXS) patterns during the electrochemical reaction of the material. Compatible with our SAXS, D8 Discover and D8 Advance aparatus.

  • Small Angle X-ray Scattering aparatus (Bruker Nanostar)

    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.
    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.

  • X-ray Powder diffraction aparatus (D8 Advance)

    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.

  • X-ray Powder diffraction aparatus (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 K-beta, K-alpha2. This minimizes 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.

SERVICES OFFERED BY THE ASSET

Measurement of phase and structural changes taking place in electrode materials during battery operation

Coupling our in-situ electrochemical cell with one of our X-ray diffraction equipments (D8 Advance, D8 Discover) or Small Angle X-ray Scattering (SAXS Nanostar) we can study changes in the morphology and crystalline structure of a material during its electrochemical reaction. This is typically used for electroactive electrode materials for secondary batteries but can also be used for the study of primary batteries as well as any electrochemical reaction.

Measurement of the microstructure (porosity, size of nanoparticles, order in disordered materials ...) at low angles

This service is based on the use of the Small Angle X-ray Scattering technique (SAXS) which allows the study of the morphology (particle size, internal or external porosity etc…) and the nanometer and subnanometer range. 2D mapping of the samples is also possible, with a micrometer resolution, in order to observe density changes and compare the SAXS measurements at various positions of a sample. SAXS requires powder sample or flat sample (typical thickness 50um-2mm depending on absorption).

ENTITY MANAGING THE ASSET

ENTITY MANAGING THE ASSET
CIC energiGUNE
Contact person:
Leire Olaeta Rodríguez
lolaeta@cicenergigune.com