RESEARCH FACILITIES

Ca. 30 lab-scale plants, for both liquid and vapour phase processes, both in batch and in continuous-flow mode, equipped with analytical facilities (on-line GC and micro GC)

 

Online GC: Agilent 6890 equipped with FID and TCD detector,

Online micro GC: Agilent 3000A. HP Plot-Q column, OV1 and Molecular sieve 5Å column

TPD-R-O (with MS)

Micromeritics Autochem II 2920 instrument coupled with a Cirrus 2 quadrupole mass spectrometer

DRIFTS (with MS)

Bruker Vertex 70 instrument equipped with a Pike DiffusIR cell attachment and a MCT detector

BET; Porosimeters.

SORPTY 1750 (Fisons Instruments)

Micrometrics ASAP™ 2020

TGA-IR, DSC.

TGA TA Instruments SDT-Q600

Ex-situ and in-situ FT-IR; ATR

ATR-IR Bruker (Billerica, MA, USA) Alpha

MS spectrometers (GC-MS, ESI)

Agilent Technologies 6890 gas-chromatographer coupled with an Agilent Technologies 5973 mass analyzer (GC-MS)

Access through the Industrial Chemistry Department “Toso Montanari” to the following facilities:

 

  • NMR spectrometers (300 mHz, 400 mHz, 600 mHz);

       Varian “Mercury 400” and “Mercury 600” spectrometers, operating at 400 and 600 MHz, respectively.

 

  • SEM-EDX;

       Microscope 50 EP (LEO ZEISS) with Oxford Instruments INCA ENERGY 350 microdetector (EDS) with INCASmartMap system

 

  • Ex-situ and in-situ Raman;

        Renishaw Raman System RM1000 equipped with Leica DLML confocal microscope, with 5x, 20x and 50x objectives,

        video camera, CCD detector and laser source Argon ion (514 nm)

 

  • X-Ray diffractometer (access to powder XRD);

       Philips PW1050/81 diffractometer equipped with a graphite monochromator and controlled by the PW1710 detection unit

       (Cu Kα, λ=0.15418 nm)

 

  • X-ray photoelectron spectroscopy (XPS);

        Kratos AXIS Supra+ (iEntrance)

Axis Supra+ is a high-performance XPS spectrometer with a high level of automation. The ultra-high vacuum (P = 5∙10^-10 torr) in the sample analysis chamber is maintained by a mechanical pump, a primary turbomolecular pump, and a secondary Ti sublimation pump. Samples are loaded into a pre-chamber (Fexi Lock) that can hold up to 3 sample holders. Once the pre-chamber reaches the correct pressure (P = 5∙10^-9 torr), the sample holders can be transferred into the SAC through a fully automated procedure that allows remote analysis.

Samples can be manipulated by an automated five-axis system (X, Y, Z, θ, Φ) equipped with permanent standards (Au, Ag, and Cu) for spectroscopic calibration and an Au grid for imaging. Different types of sample holders are available.

- General-purpose sample holder (90 x 32 mm) for samples up to 14.5 mm in thickness.
- Sample holder with electrical connections and station for electrochemical analysis for in situ experiments on devices with solid-state electrolyte (iEntrance accessory not included).
- Sample holder with Z rotation: primarily used in profilometric analysis experiments.

A color camera in the pre-chamber provides an overall view of each sample holder for indexing and programming an analysis position sequence. For further position selection, a high-magnification microscope controlled by software with a 12x motorized optical zoom system is used in the SAC.

A dual anode Ag/Al X-ray source provides Al Ka monochromatic radiation (1486.7 eV) for XPS or Ag Ka radiation (2984.3 eV) for HAXPES, both focused on the same analysis position. The exchange between excitation sources and repositioning of the monochromator (Rowland circle) is fully automated and computer-controlled.

The Delay Line Detector (DLD) is used for both spectroscopy and imaging. The DLD has three operating modes: traditional scanning spectroscopy mode, fast (less than 1 second) non-scanned spectroscopy acquisition mode (snapshot mode with 128 data channels), and parallel two-dimensional imaging mode (spatial resolution at maximum magnification = 1 μm).

XPS spectroscopy of selected areas is achieved with a plate featuring a series of precision apertures, for both large areas (700x300 μm slit) and small points (diameter = 110 μm, 55 μm, 27 μm, or 15 μm).

The analysis areas in parallel imaging mode can reach up to 400x400 μm; larger images (up to 10x10 mm) are available through "imaging stitching," combining the sample holder movement controlled by the software with parallel imaging.

An integrated charge neutralizer provides a low-energy electron beam for neutralizing insulating samples during the photoemission process.

A monoatomic Ar+ ion source “Minibeam 4” with energies ranging from 0.5 to 4 keV and a rating from 0.5 to 4 keV operates in floating mode for sample surface sputtering/cleaning and depth profiling experiments.

A programmable high-temperature reaction cell is available, with temperature and pressure control, compatible with H2, O2 air, N2, H2O, CO2, and CH4. It can be used for ex situ analysis on up to 4 samples simultaneously. The maximum operating temperature is 1000 °C at 0-10 bar, 800 °C at 10-20 bar, and 300 °C at 20-30 bar.

The instrument will also be equipped with an accessory for ultraviolet photoelectron spectroscopy (UPS) - He arc lamp (iEntrance accessory not included).

 

  • XRF analyser;

       PANalytical Axios Advanced WD-XRF spectrometer equipped with a Rh-anode X-ray tube (maximum power = 4 kW)

 

  • AAS (atomic absorption); MP-AES (microwave plasma - atomic emission spectrometry)

       Agilent 4210 MP-AES instrument

 

  • DLS; VCD-ECD;

      DLS and electrophoretic light scattering ELS measures, registered by using a Malvern Panalytical

      (Malvern, United Kingdom) Zetasizer Nano ZS instrument.

 

  • Computer centre (about 500 processors)