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Multi-Functional Nanomaterial Group

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The research group is characterized by unique competences in the whole DiSC department on the design and fabrication of multifunctional inorganic nanoarchitectures by means of vapor phase routes.

The research activities of the group cover the design and synthesis of suitable metalorganic/coordination precursors for the target nanosystems and their detailed characterization (XRD, IR, NMR, mass spectrometry, theoretical calculations,…), even in the framework of external collaborations.

The currenty adopted nanosystem preparation processes encompass chemical vapor deposition (CVD), both thermal and plasma-enhanced (PE-CVD), Radio Frequency (RF)-Sputtering, and original hybrid approaches to develop multi-component nanosystems with tailored chemico-physical properties. The related synthesis facilities include:

These reactors have been originally designed developed and implemented by the research group members.

Afterwards, the nanosystem fabrication by the above described processes is constantly accompanied by a multi-technique chemico-physical characterization, enabled by the forefront instrumental equipment and related know-how in the analysis of nanomaterial structure, morphology and composition. These activities provide a key background for the optimization of the above discussed synthetic protocols as a function of the ultimate material applications.

The commonly used in-house characterization techniques include:

- a cold-wall thermal CVD apparatus, dedicated to the synthesis of low-sized (1×1 cm2) specimens;

- a hot-wall thermal CVD reactor, equipped with an FT-IR spectrometer to monitor in real time the gas phase composition during the process, enabling the processing of larger substrates (up to 5×5 cm2);

- a plasma-assisted reactor for PE-CVD and RF-sputtering experiments, equipped with a laser reflection interferometer (LRI) for the on-line diagnostics of growth processes.

- electrophoretic deposition (EPD) to finely tune the degree of functionalization of the substrate for the improvement of its properties by exerting a direct control of various parameters (voltage, time, current, electric field homogeneity, etc.).

X-ray Diffraction (XRD), to investigate the system microstructural characteristics and obtain information on crystalline phases, as well as anisotropy/preferential orientation effects;

X-ray Photoelectron Spectroscopy (XPS), X-ray Excited Auger Electron Spectroscopy (XE-AES) and Ultraviolet Photoelectron Spectroscopy (UPS), for the study of elemental composition, chemical state of the different species and their surface and in-depth distribution;

Atomic Force Microscopy (AFM) and Field-Emission Scanning Electron Microscopy (FE-SEM), for the analysis of the surface morphology and three-dimensional organization, as well as Energy Dispersive X-ray Spectroscopy (EDXS) analyses;

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Optical spectroscopies (IR, UV-Vis, …) for the analysis of functional groups and of the system band-gap energy;

Microbalance for the estimation of the nanomaterial weight.

The group is also equipped with two multi-purpose workstations for the functional (photo)electrochemical characterization of the developed materials in view of their use as (photo)electrodes for water splitting and photoelectrocatalysts for pollutant degradation. These instruments allow both standard material electrochemical characterization (linear scanning voltammetry (LSV), electrochemical impedance spectroscopy (EIS)] and advanced analyses based on intensity modulated photocurrent spectroscopy/photovoltage spectroscopy (IMPS/IMVS) and incident photon conversion efficiency (IPCE). In particular, the Zahner photoelectrochemical system allows a continuous real-time measurement of the light intensity illuminating the sample.

In the framework of external scientific cooperation, the target nanomaterials are also chatacterized by:

• Secondary Ion Mass Spectrometry (SIMS), for the analysis of the in-depth system composition, of segregation phenomena and of possible material-substrate interdiffusion processes;

• Transmission Electron Microscopy (TEM), High Resolution-TEM (HR-TEM), High Angle Annular Dark Field-Scanning TEM (HAADF-STEM), for an advanced study of the system nanostructure as a function of the processing conditions, supported by Electron Energy Loss Spectroscopy (EELS) to analyze the local composition and the mutual distribution of the various phases in the synthesized composites.