ANALYTICAL CHEMISTRY OF SURFACES AND INTERPHASES
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
Knowledge of instrumental analytical chemistry
Course contents summary
The class will overview the analytical aspects related to interphases and surface study.
Within the course applicative examples will be provided concerning up-to-date technologies currently used in chemical, electronics and mechanical industry.
The outline of the course is as follows:
-Interphase and surface definition
-Classic and modern methods for interphases study
-Selective and non selective chemical etchings
-Layer deposition techniques
-Surface and interphases characterization
-Fundamentals of electron spectroscopies
- Ion spectroscopies
-Fundamentals of ellissometry
-Techniques for nanoparticles determination
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
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.
Selective and non-selective chemical etchings.
Composition rules for the etching mixtures, ternary composition
diagrams, viscosity and temperature effects.
Photoactivated chemical etchings.
Physical Vapour Deposition and Chemical Vapour Deposition.
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.
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
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
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.
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-
Lectures and exercitations
Assessment methods and criteria
verbal examination of 30 min as an average. 3 questions will be proposed to the candidate. Further questions will be proposed if there is a no-answer up to 5 questions. the evaluation will be given taking in account the comprehension and personal further study of the questions proposed, according to the following scheme: full comprehension and additional personal study of all the 3 questions: 30 com laude, excellent comprehension in all the 3 questions:28-30, good comprehension in all the 3 questions or excellent in 2 and reasonable/sufficient in 1: 27-26, reasonable in all the 3 questions or good in al least 2: 25-23, sufficient in all 3 or reasonable in at least 2: 22-18. For no answer there will be a penalty of 2-3 points