GISEL (National Centre of Reference for Electrochemical Energy Storage Systems)

Equipment and instrumentation of GISEL

All the Research Units have the standard equipment and instrumentation for the assembly and electrochemical tests of half-cells and complete cells with two and three electrodes (high-performance glove-boxes, potentiostats/galvanostats, multichannel cyclers for batteries also with booster). This general equipment and instrumentation will therefore not be detailed, except in the case of systems with particular characteristics. In the following, the main equipment and instruments available will be grouped by category, highlighting the most significant characteristics and indicating the reference Research Unit.

1) EQUIPMENT FOR THE SYNTHESIS OF MATERIALS AND THE MANUFACTURING OF DEVICES

  • Environmental chambers from -40°C to 180°C in a controlled atmosphere (Milano Bicocca, Camerino, Turin Polytechnic, Chieti-Pescara).
  • 10 m2 dry-room for the manufacture of prismatic cells (Turin Polytechnic)
  • 11 mm co-rotating twin screw extruder (Thermo Haake) with 8 temperature-controllable zones, and two inputs with volumetric feeding. It allows to combine thermoplastic polymers and micro or nanometric additives, obtaining batches for subsequent use. The total flow rate is between 1 and 2 Kg / h depending on the polymer used (Milano Bicocca)
  • Electron beam evaporator with semi-automatic wire bonder complete with heated stage and microscope (Milano Bicocca)
  • Furnaces (also in controlled atmosphere and vacuum) for solid-state synthesis of ceramic materials (Milano Bicocca, Pavia, Padua, Turin Polytechnic, Bologna)
  • Dedicated lines for the manufacture of coin cells and pouch cells (Padua)
  • Multifunction microwave ovens for chemical synthesis (Turin Polytechnic, Bologna, Pavia)
  • Electrospinning systems (Chieti-Pescara, Pavia)
  • CAD/CAM system (Padua)
  • System for the deposition of liquid-based suspensions following a predetermined two-dimensional design by means of a numerical control system piloted by a computer. The system, designed for industrial applications, has a camera to follow the deposition process and a heated vacuum table (Padua)
  • Spin-coating systems (Pavia, Padua)
  • Plasma deposition systems (DC and RF sputtering) (Padua, Pavia)
  • UV systems with optical fiber for photo-polymerization (Turin Polytechnic)
  • 3D wire printers for polymeric, ceramic, composite, powders and colloidal suspensions (Milano Bicocca, Pavia)
  • Fritsch and Retsch planetary mills with jars of various materials (Milano Bicocca, Padua, Pavia, Bologna, Chieti-Pescara).

2) INSTRUMENTATION FOR THE CHARACTERIZATION OF MACROSCOPIC PROPERTIES (HEATS OF REACTION, WEIGHT, DENSITY, MECHANICAL MODULES, VISCOSITY, SURFACE AREA, CONDUCTIVITY, ETC.)

  • Dynamic-mechanical analyzer DMA 25 Acoem/Metravib (Calabria)
  • TA Instruments dynamic-mechanical analyzer between -150 and 600°C, equipped with various accessories, including the "Dual / Single Cantilever" (for the study of thermoplastic materials), the "compression clamp" (for materials with low to moderate) and the "tension clamp" (for fibers and films) (Padua)
  • Dynamic Light Scattering Particle Analyzer (Bologna)
  • Surface area analyzers using N2 adsorption isotherm (BET) (Padua, Pavia, Rome)
  • Apparatus for measuring the Hall effect operating between 20 and 350 K (Milano Bicocca)
  • Differential Scanning Calorimetry (DSC) also modulated up to 700 C (TA Instruments, Mettler Toledo) (Pavia, Padova, Milano Bicocca)
  • Micro-DSC Calorimeter Setaram (Calabria)
  • Broadband Electrical Spectroscopy (BES) lines. Various tools and accessories are available that allow to determine the electrical properties (eg permittivity, conductivity, etc.) of solid and liquid materials. The available instrumentation allows to determine these electrical properties as a function of frequency (from 10-4 to 20 GHz), temperature (from -140 to 220 ° C), gas pressure (from 0 to 150 bar) and relative humidity (from 0 99%) (Padua).
  • Electrochemical Impedance Spectroscopy (EIS) lines. Typical frequency range between 10-2 Hz and 107 Hz. Supplier companies: Schlumberger, Biologic, Ecochemie, etc. (Milano Bicocca, Padua, Pavia, Turin Polytechnic, Bologna, Camerino, Rome, Calabria).
  • Pycnometer (Padua)
  • Porosimeter with kit for micropores (Bologna)
  • Mechanical profilometer Tencor (Pavia)
  • Anton Paar rheometer with parallel plate geometries and concentric cylinders, water temperature control, contactless electric motor with compressed air (Milano Bicocca)
  • Shear-strain controlled rheometer (Rheometer RFS-III) and Shear-stress controlled rheometer DSR5000 (Rheometrics Scientific) (Calabria)
  • High resolution TGA Ta Instruments (Padua, Pavia, Bologna, Turin Polytechnic)
  • TGA/DSC Mettler Toledo coupled with MS Thermostar mass analyzer (Milano Bicocca)
  • TG/FTIR (Milano Bicocca)

3) INSTRUMENTATION FOR THE CHARACTERIZATION OF STRUCTURAL AND MICROSTRUCTURAL PROPERTIES (DIFFRACTION, MICROSCOPY, SPECTROSCOPY) AND CHEMICAL COMPOSITION

  • CHNS-O Elementary Analyzer (Milano Bicocca, Padua)
  • X-ray diffractometers for powders and/or thin films, also in controlled atmosphere, in situ and with sample heating systems up to 1000 ° C (Milan Bicocca, Bologna, Padua, Pavia, Rome, Reggio Calabria)
  • X-ray diffraction and fluorescence (Mo source + position sensitive detector) for structural and chemical analysis of materials (Calabria)
  • AFM microscopes (Pavia, Reggio Calabria)
  • FESEM ZEISS SIGMA 300 microscope with Gemini column, max resolution of 1.2 nm @ 15.0 kV. High efficiency "in-lens" secondary electron detector; ETSE secondary electron detector; HDBSD backscattered electron detector with 4 independent sectors. Microanalysis system with SDD Bruker Quantax 200 technology with LN2-free cooling, characterized by a resolution of 129 eV @ 5.9 keV (Mn k-alpha) (Camerino).
  • SEM and Hi-Res SEM microscopes with EDX (Milano Bicocca, Pavia)
  • TEM microscopes with columns up to 200 kV (Milano Bicocca, Reggio Calabria)
  • ESR Bruker EMX spectrometer with Oxford cryostat and vacuum system (Milano Bicocca)
  • FTIR and ATR-FTIR spectrometers (Biorad FTS6000, Bruker Vertex 70v with specular reflection and MIR, Bruker Alpha) (Milano Bicocca, Padua, Rome)
  • High and low power confocal micro-Raman spectrometers (Padua, Milan Bicocca, Rome, Reggio Calabria)
  • Horiba micro-Raman spectrometer with double laser source (532 nm/633 nm), double Olympus optical microscope, cell for electrochemical characterizations, cell for 80-600K variable temperature measurements (Camerino)
  • Multifunctional spectrometer SPM NTEGRA, confocal Raman with SERS, SNOM, nanofluorescence and STM (Scanning Tunneling Microscopy) capability (Reggio Calabria)
  • Multinuclear solid-state spectrometer MAS-NMR 400 MHz Brukerc with functional microimaging (Milano Bicocca)
  • Bruker 300 MHz NMR spectrometer with diffusion accessory (Calabria)
  • Bruker Minispec mq20 NMR relaxometer 20 MHz with nitrogen flow temperature control (between -100°C and 200°C) . The instrument is also equipped with a gradient unit to measure the diffusion coefficient of molecules in a fluid, a gel or a porous solid (Milano Bicocca)
  • High resolution 200 MHz and 500 MHz NMR spectrometers (Padua, Milano Bicocca)
  • Low-vacuum XPS spectrometer (Near-Ambient Pressure X-ray Photoelectron Spectrometer, NAP-XPS). This instrumentation allows to study the composition and the surface chemical state of both insulating and electrical conducting samples. It is possible to work up to pressures of 10-30 mbar to characterize liquid or semi-solid samples (Padua)
  • Atomic Absorption Spectroscopy AA-6300 (Calabria)
  • Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) . Two ICP-AES instruments are available which allow to determine the composition of samples after their mineralization. It is possible to simultaneously determine the concentration of the elements even if the latter are present in traces (some ppb). These instruments are able to detect the presence of almost all the elements of the periodic table, with the exception of rare gases and very light elements such as H, C, N and O (Padua)
4) COMPUTATIONAL METHODS

  • Local clusters of various sizes are available in addition to access to national computing centers (e.g. Cineca) (Naples, Milan Bicocca, Pavia, Milan Polytechnic)

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