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Pavia H2 Lab

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University of Pavia

Department of Chemistry / Physical Chemistry Section

The Research activity of the Pavia H2 Lab (http://h2lab.unipv.it) at the Physical Chemistry Section of the Chemistry Department of the University of Pavia mainly regards the preparation and the characterization of nanomaterials for solid state hydrogen storage. The preparation is made in bulk form by high energy ball milling or as nanoscaffolds (the hydrides are dispersed–encapsulated in high surface area porous matrices) by wet chemistry.

The lab is equipped with "state of the art" instruments allowing to perform all the measurements suggested by the US Department of Energy (DoE) for the H2 storage systems characterization.

Facilities

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Glove-box (MB-Braun) for samples handling and storage under Ar (O2 and H2O levels <0.1 ppm).
bullet-blue-s2 Planetary milling machines (Fritsch) and vials for the preparation of the samples by high energy ball milling both under inert atmosphere (Fritsch) and under H2 (up to 150 bar – Evico Magnetics), with in situ temperature and pressure measurements.
bullet-blue-s2 Manometric Sievert type apparatus (Hy-Energy PCT-Pro 2000), operating in the T range -196÷500 °C and in the H2 pressure range 10-3÷200 bar.
bullet-blue-s2 Residual gas analyzer (RGA-Pro) designed to work with the PCTPro-2000 for real-time compositional analysis of sorption gases from the sample chamber. The system uses a 200 amu quadrupole mass spectrometer with resolution better than 1 amu. It can work up to 200 bar and 500 °C.
bullet-blue-s2 High–Pressure Differential Scanning Calorimeter (Setaram Sensys), covering the temperature range 18÷600 °C and the H2 pressure range 10-6÷180 bar. The system can work in isobaric conditions and with controlled scanning pressure rates thanks to an ad hoc gas panel projected by the Pavia group and realized by Setaram. The instrument can work coupled with both the manometric instrument and the RGA. The Pavia group was the first in Europe to realize the couplement between the manometric and the calorimetric instrument and to publish coupled kinetic-calorimetric data.
bullet-blue-s2 Scanning Electron Microscope (Zeiss EVO MA10-HR) with energy-dispersive microprobe analyzer (Oxford INCA Energy 350X Max). The Pavia research group has developed and realized a special chamber to avoid the oxygen contamination of the powders before and after the SEM measurements.
bullet-blue-s2 Tubular ovens inside the glove box able to work up to 1000 °C for the thermal treatments of the samples and the preparation of the sorption intermediates for the ex-situ analyses.
bullet-blue-s2 X-ray powder diffractometer (Bruker D5005) with a polythermal chamber operating under controlled atmosphere from -170 °C up to 1100 °C. The Pavia group has at its own disposal a special air tight sample holder for measurements of very low amount of samples (few mg) under inert atmosphere at room temperature.
bullet-blue-s2 Porosimeter (ThermoScientific Sorptomatic) for the analysis of the surface area of the powders (B.E.T. method, analyzing gas: N2; working T = -196 °C).
bullet-blue-s2 Thermal conductivity analyzer (TCI, C-Therm) able to work up to 200 °C (heating of the sensor + the sample by a band heater). The sensor has been placed in the glove box to enable measurements on air sensitive samples. the system is unique and very original.

Thanks to the collaboration with the University of Barcelona, High Resolution-TEM measurements can be performed.

Moreover, thanks to collaboration with HZG in Germany, in situ and ex situ Raman measurements (up to 600 °C under H2 atmosphere) and anisotropic thermal conductivity measurements will be performed.

The AFM-NMR Laboratory of the University of Milano will perform high sensitive in situ and ex situ NMR measurements.