ANALYTICAL CHEMISTRY OF SURFACES AND INTERPHASES
cod. 08919

Academic year 2017/18
2° year of course - First semester
Professor
MUCCHINO Claudio
Academic discipline
Chimica analitica (CHIM/01)
Field
Discipline chimiche analitiche e ambientali
Type of training activity
Characterising
48 hours
of face-to-face activities
6 credits
hub: PARMA
course unit
in ITALIAN

Learning objectives

At the end of classes the student should be able to:
-knowledge and understanding the basic concepts of reactivity and properties of surfaces and nanoparticles
-knowledge of the main techniques aimed at building interphases with requested characteristics both physic-chemical and functional
-being familiar with the most relevant characterization techniques of surfaces, interphases and nanoparticles
-understanding the production processes used in new material fabrication such as Swarovski crystal, multilayer lenses composite and multilayer materials used in chemical, electronic and mechanic industry
-making judgment about and put forward the analytical technique to achieve the best results, taking in account performance, costs, and time spent.
-being able to hyphenate various analytical techniques with the purpose of obtaining new possibilities in interphases and nanoparticles characterization

Prerequisites

Knowledge of instrumental analytical chemistry

Course unit content

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.

Full programme

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.

Bibliography

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. Due to the innovative and advanced nature of the topics, and having to condense many interdisciplinary knowledge It is strongly recommended to students to attend classes and to take their own notes. The suggested textbooks may be too dispersive or not covering the most advanced topics. As well as classic topics are concerned, slides will be provided while for the advanced topics the classical blackboard lesson will be given and the provided material will concern supplementary information only or a scientific paper to be discussed.

Assessment methods and criteria

an oral test with critical discussion concerning at least 3 main course topics (surface preparation and definition, analytical techniques, nanoparticles techniques). The student should demonstrate the understanding of the topics and their application, with the examiner support, even to cases not specifically discussed during classes. The result will be immediately notified to the student.

Other information

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