ANALYTICAL CHEMISTRY OF SURFACES AND INTERPHASES

Teachers: 
Credits: 
6
Site: 
PARMA
Year of erogation: 
2020/2021
Unit Coordinator: 
Disciplinary Sector: 
Analytical Chemistry
Semester: 
First semester
Language of instruction: 

italian

Learning outcomes of the course unit

To provide the fundamental concepts on the properties and reactivity of
surfaces, with reference to the new
materials. Highlights the main analytical techniques for interphases and
surface characterisation and their
proper use.

Prerequisites

Knowledge of instrumental analytical chemistry

Course contents summary

Definition of interphase and surface, bulk and (multi)layers materials
Classification of interphases
Classical and modern methodologies for the interphase characterisation:
application field and information
obtained.
Thickness of the interphase region.
Application fields: examples of reaction, processes and phenomena that
involve the interphase concept.
Classification and main properties of interphases.
Surface preparation and modification, etching and deposition techniques.
Etching techniques.
Selective and non-selective chemical etchings.
Composition rules for the etching mixtures, ternary composition
diagrams, viscosity and temperature effects.
Photoactivated chemical etchings.
Deposition techniques
Physical Vapour Deposition and Chemical Vapour Deposition.
Characterization.
Morphological characterisation of interphases: point, surface, localised
and extended defects, defect
propagation within the interphase.
Chemical characterisation of interphases: compositional inohomogeneity
Evaluation of functional characteristics.
Characterization techniques.
Interactions betweens particles and matter. penetration in the
interphase, diffusion and retrodiffusion
Lateral and axial diffusion.
Optical microscopy, metallographic microscope, illumination systems,
fundamental parameters of optical
microscopy, optical aberrations, bright and dark field microscopy,
polarised and monochromatic light
microscopy.
Combined use of optical microscopy and chemical etchings.
Quantitative analysis in optical microscopy, fundamentals of data
acquisition and image digitalization
systems, expert and non expert automatic recognition systems
Scanning Electronic Microscopy, basic instrumentation and working
principle, maximum magnification, sample
characteristics, limitations and sample preparation, detectors
Combined use of SEM, X-ray fluorescence and Auger electron
spectroscopy.
Atomic force spectroscopy and profilometers.
Fundamentals of X-ray fluorescence, microprobe, the energy dispersive
detector, applicative examples
Fundamentals of Auger electron spectroscopy, principles and
instrumentation, application field and comparison
with x-ray fluorescence, compositional profiles, examples and applications.
Fundamentals of other electron spectroscopies: ESCA, UPS.
Laser ablation inductively coupled plasma mass spectroscopy LA-ICP-MS.
The secondary ion mass spectroscopy (SIMS), principles and instrumentation, ion sources, qualitative and quantitative analysis, standard preparation, concentration profiles, repeatability problems.
Ellipsometry, principles and instrumentation, the spectroscopic ellipsometry, uses of the information obtained, data acquisition and handling.
Nanoparticles determination techiques: one particle ICP-MS, fractionation techniques bidimensional calibration strategies.

Course contents

Definition of interphase and surface, bulk and (multi)layers materials
Classification of interphases
Classical and modern methodologies for the interphase characterisation:
application field and information
obtained.
Thickness of the interphase region.
Application fields: examples of reaction, processes and phenomena that
involve the interphase concept.
Classification and main properties of interphases.
Surface preparation and modification, etching and deposition techniques.
Etching techniques.
Selective and non-selective chemical etchings.
Composition rules for the etching mixtures, ternary composition
diagrams, viscosity and temperature effects.
Photoactivated chemical etchings.
Deposition techniques
Physical Vapour Deposition and Chemical Vapour Deposition.
Characterization.
Morphological characterisation of interphases: point, surface, localised
and extended defects, defect
propagation within the interphase.
Chemical characterisation of interphases: compositional inohomogeneity
Evaluation of functional characteristics.
Characterization techniques.
Interactions betweens particles and matter. penetration in the
interphase, diffusion and retrodiffusion
Lateral and axial diffusion.
Optical microscopy, metallographic microscope, illumination systems,
fundamental parameters of optical
microscopy, optical aberrations, bright and dark field microscopy,
polarised and monochromatic light
microscopy.
Combined use of optical microscopy and chemical etchings.
Quantitative analysis in optical microscopy, fundamentals of data
acquisition and image digitalization
systems, expert and non expert automatic recognition systems
Scanning Electronic Microscopy, basic instrumentation and working
principle, maximum magnification, sample
characteristics, limitations and sample preparation, detectors
Combined use of SEM, X-ray fluorescence and Auger electron
spectroscopy.
Atomic force spectroscopy and profilometers.
Fundamentals of X-ray fluorescence, microprobe, the energy dispersive
detector, applicative examples
Fundamentals of Auger electron spectroscopy, principles and
instrumentation, application field and comparison
with x-ray fluorescence, compositional profiles, examples and applications.
Fundamentals of other electron spectroscopies: ESCA, UPS.
Laser ablation inductively coupled plasma mass spectroscopy LA-ICP-MS.
The secondary ion mass spectroscopy (SIMS), principles and instrumentation, ion sources, qualitative and quantitative analysis, standard preparation, concentration profiles, repeatability problems.
Ellipsometry, principles and instrumentation, the spectroscopic ellipsometry, uses of the information obtained, data acquisition and handling.
Nanoparticles determination techiques: one particle ICP-MS, fractionation techniques bidimensional calibration strategies.

Recommended readings

T.G. Rochow and E.G. Rochow, An introduction to microscopy by means
of Light, Electrons, X-ray or ultrasound
- Plenum press NYC ISBN 0-306-31111-9
Surface and Thin film analysis: principles, instrumentation, applications;
H. Hubert and H. Jenett eds -
Wiley-VCH Verlag, Weinheim (D), electronic ISBN 3-527-60016-7
R. Kellner J.M. Mermet, M. Otto, H.M. Widmer (Eds), Analytical Chemistry
(chapter 10) - Wiley-VCH (ISBN 3-
527-28881-3)

Teaching methods

Lectures and exercitations

Assessment methods and criteria

verbal examination