<em>PADUA</em>

The seat carries out research and technology transfer in different areas of chemistry, materials and energetics

VISIT

PADUA PADUA
Headquarter

<em>MILAN</em>

Research activity in Milan concerns the properties and technology of structural and functional materials, fluid dynamics, and diagnostics or reactive systems.

VISIT

MILAN MILAN
Organizative Unit

<em>GENOA</em>

ICMATE-Genoa has expertise in the fields of physical chemistry of interfaces and in the preparation of powders, ceramics and composites of functional oxides.

VISIT

GENOA GENOA
Organizative Unit

<em>LECCO</em>

ICMATE-Lecco is one of the few centers in Italy able to operate in the secondary metallurgy of advanced metallic materials

VISIT

LECCO LECCO
Organizative Unit

The laboratory is focussed on microstructural investigations of solid materials through high-resolution scanning electron microscopy (SEM microscope, Fig. 1), with:

  • in-chamber detectors for conventional observations with secondary electrons (SEI) and backscattered electrons (BEI) (Fig. 3a) for surface observations of bulk materials;
  • in-column detectors for high resolution investigations; detector dedicated to observations of thin foils through scanning transmission electron microscopy (STEM) to investigate the inner microstructure of materials (Fig.s 2a and b);
  • a system for micro-analytical semi-quantitative analysis through energy dispersive spectroscopy (EDS) with last generation LN-free SDD detector with improved energy resolution and high acquisition rate (up to 100,000 cps) for elemental maps with high spatial resolution (Fig. 3b);
  • an acquisition system of Kikuchi electron backscattered diffraction (EBSD) patterns for surface crystallographic mapping with high spatial resolution (Fig.s 4a and b).

The laboratory is outfitted also with conventional metallographic optical microscopy (OM) and X-ray Bragg-Brentano diffraction system (θ-2θ) for crystallographic characterization of polycrystalline materials and characterization of the deformation state and residual stresses of materials.

The laboratory is equipped with chemical instrumentations for specimen preparation related to the described analysis techniques.

  • EQUIPMENT:
    • Metallographic optical microscope Leitz DM RNE;
    • High resolution scanning electron microscope SU-70 Hitachi (resolution limit = 1.6 nm) with:
      • Conventional in-chamber detectors for secondary (E-T) and solid state detector for backscattered electrons;
      • High resolution in-column detectors for secondary and backscattered electrons with energy filter;
      • Scanning transmission electron detector (STEM);
      • Micro-analitical system Noran 7 by ThermoScientific Inc. for energy dispersion spectroscopy (EDS) with LN-free SDD detector;
      • Micro-analitical system Noran 7 by ThermoScientific Inc for electron back scattered diffraction (EBSD) acquisition and analysis;
    • X ray diffraction system Siemens D500;
    • Instrumentation for metallographic preparation;
    • Twin jet Tenupol by Struers for electro-polishing for thin foil preparation for STEM observations.
    • Fiber-coupled diode laser: Laserwave 250 W - 980 nm
Fig. 1 – HR SEM microscope SU70 – Hitachi.

Fig. 2 – STEM micrographs: (a) multi-walled nanotube; (b) dislocation-precipitate interactions in stainless steel AISI 441.

Fig. 3 – (a) BEI micrograph of Ag-Cu-Si produced by rapid solidification (RS); (b) elemental map of (a).

Fig. 4 – (a) EBSD orientation map of stainless steel AISI 304 deformed at 1100°C, 10-1 1/s; (b) dislocation structure of (a).
  • A Field Emission Scanning Electron Microscope (FE-SEM) can perform morphological investigation of samples having various morphologies and characteristics. In fact, various materials have been analyzed so far: metals, ceramics (alumina, zirconia, composites, advanced ceramics for ionic conduction, etc.), coatings and various samples having different size and composition also as service for industries or other labs. The FE-SEM is equipped with EDS detector for compositional analysis and mapping. Furthermore, a heating stage (up to 800°C) inside the chamber of analysis allows morphological observations in temperature.
    To analyze insulating materials a deposition of a very thin metal coating can be assured by PVD.


    • EQUIPMENT:
      • FE-SEM Sigma Zeiss
      • EDS Oxford X-MAX
      • Tavolino riscaldante Kammrath & Weiss

  • The laboratory is equipped with a Field Emission Scanning Electron Microscope (FESEM) FEI Quanta 200F (FEI), operating also in low vacuum, which allows the direct investigation of the sample or as cross section. A SEM analysis provides information concerning sample morphology at micro and nanoscale level and surface composition. The images are obtained by means of secondary or back-scattered electrons (SE or BSE respectively) analysis. The microscope can also provide structural information by the investigation of back-scattered electron diffraction (EBSD) followed by software data processing and compositional information by X-ray spectrometry analysis also combined with BSE imaging.

    Fig. 1) FEI Quanta 200F

    In the same laboratory three optical microscopes are also available. In detail: Olympus SZX12, Olympus BX51 and Leitz Ergolux allow the direct investigation of the sample or as cross section , providing coloured 3D images (stereo-microscopy) or 2D (classic optical microscopy). The optical microscopes can also operate with a digital camera or with a PC interfaced camera, thus allowing the direct storage of HD images of the sample.


    Fig. 3) Olympus SZX12
    Fig. 4) Leitz Ergolux
    • EQUIPMENT:
      • FEI Quanta 200F
      • Olympus SZX12
      • Olympus BX51
      • Leitz Ergolux

The metallographic laboratory enables for the preparation of metallic and ceramic specimens for the observation/analysis with both optical or electronic microscope.


The system SEM + EDS + IA (Image Analysis, Auto ­ Soft Imaging System) allows for the observation of conducting and/or insulating and biological samples, to perform localized qualitative and quantitative analyses, starting from Boron. Image analysis provides dimensional information.

  • EQUIPMENT:
    • Specimens preparation
      • Semiautomatic polishing machines;
      • Vibrating Bühler VIBROMET polishing machine;
      • Sputtering machines;
      • Diamond saw cutting machines.

    • Microscopy
      • Variable Pressure Scanning Electron Microscope (VP-SEM) equipped with backscattered electrons detector and EDS microanalysis;
      • Metallographic optical microscope ZEISS AX10;
      • Optical microscopy system for the study of emulsions.

The laboratory of Microstructural Characterization groups the instrumentations for metals and crystalline material characterization.
Two Scanning Electron Microscopes (SEM) are available for morphological studies, allowing investigation from millimeter to nanometer size: fracture surfaces, external appearance, inclusions as well as other microstructural features can be observed. Optical microscopes are also available to support sample observation before SEM analyses.
SEMs are equipped with Back Scattered Electron (BSE) and Energy Dispersive X-ray Spectrometry (EDS) detectors for qualitative and semi-quantitative chemical analyses, and EBSD (Electron Back Scattered Diffraction) detector for phase identification and texture analyses on microscopic scale.
An XRD diffractometer is also available for crystallographic studies on macroscopic scale. The instrument can be equipped with two non-ambient temperature chambers, allowing crystallographic analyses and phase transformation studies between -180°C and 1200°C.
The laboratory facilities are completed by a set of instrument for specimen cutting, mounting, grinding and polishing and other operations in order to obtain the required conditions for the different microstructural analyses.

Hitachi SU70 – FEG SEM

High magnification trasmission micrograph: precipitates in aluminum alloy

Micrograph of electrolitic nickel powder
EBSD analysis example: twins in Ni-alloy

X’Pert PRO MPD diffractometer
Xray diffraction study of microstructural evolution of a sample subjected to thermal treatment
  • EQUIPMENT:
    • Scanning Electron Microscope Hitachi SU-70 (FEG-SEM) for high resolution imaging, equipped with:
      • Conventional in-chamber detectors for secondary (E-T) and solid state detector for backscattered electrons;
      • High resolution in-column detectors for secondary and backscattered electrons with energy filter;
      • Scanning transmission electron detector (STEM);
      • Micro-analitical system for energy dispersion spectroscopy (EDS) with LN-free SDD detector;
      • Micro-analitical system for electron back scattered diffraction (EBSD) acquisition and analysis.

    • Scanning Electron Microscope (SEM LEO 1430) with tungsten source, with secondary and back-scattered electron detectors, Energy dispersive X-ray spectroscopy (EDS) Oxford INCA Energy and Electron Back-Scattered Diffraction (EBSD) INCA Crystal.

    • Metallographic light microscope Aristomet equipped with polarizing filter.

    • Stereo-microscope equipped with LED lighting and polarizing filter.

    • Micro-indenter Leitz Miniload.

    • X-ray Powder Diffractometer, Panalytical XPert PRO MPD with θ-θ alignment, equipped with:
      • X'Celerator linear detector;
      • Non-ambient temperature chamber Anton Paar TTK-450 (-190/+450°C) and Anton Paar HTK 1200N(25°C/1200°C);
      • Spinner for phi scan measurements.

    • Instruments for metallographic preparation: metallographic diamond saw, grinding and polishing equipment, hot mounting press, sputter.

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