ADVANCED METHODOLOGIES FOR THE SYNTHESIS AND CHARACTERIZATION OF NANOSTRUCTURED MATERIALS

Academic Year 2025/2026 - Teacher: GRAZIELLA MALANDRINO

Expected Learning Outcomes

The course's main educational objective is to develop knowledge in the synthesis and characterization of materials in the form of thin films, ultrathin films, and nanostructured systems using advanced methodologies.

  • Knowledge and understanding: To acquire theoretical and experimental knowledge of the synthetic procedures of materials in the form of films, ultrathin films, and nanostructured systems
  • Knowledge and understanding: To acquire knowledge on the main structural characterization techniques, morphological, and compositional materials.
  • Applying knowledge and understanding: Ability to apply what students have learned during the lectures on the synthesis and characterization of materials in the experiments carried out in the laboratory.
  • Making judgments: Students learn to evaluate in an objective way how much they understand the lectures and the laboratory activities.
  • Communication skills: Students acquire communication skills that are developed both during lectures and lab activities thanks to a continuous verbal dialogue with the teacher, and furthermore during the oral exam.
  • Learning skills: Learning skills are assessed through oral examination and laboratory reports, which are an important part of the course.

Information for
students with disabilities and/or learning disabilities
To ensure equal opportunities and in compliance with applicable laws, interested students may
request a personal interview, allowing for the planning of any compensatory measures tailored to their educational objectives and specific needs.

 

Course Structure

Teaching will be done through lectures. 

Required Prerequisites

Basic knowledge of inorganic chemistry and basic solid state concepts.

Attendance of Lessons

Attendance of lessons is required in accordance with the regulations of the CdS.

Detailed Course Content

Frontal lessons (6 CFU)


Atomic layer deposition (ALD)

- Theoretical principles: temporal ALD and spatial ALD

- Case studies: simple oxide deposition (Al2O3); photonic crystal synthesis; deposition of multi-component systems.

Chemical Vapor Deposition (CVD) and Metal-Organic-CVD (MOCVD)

- Theoretical principles: transport phenomena; mechanisms and reaction kinetics; nucleation and growth.

- Case studies: deposition of simple oxides and multi-component oxides; fluoride film deposition.

- Processes of industrial interest: deposition of GaN, AlN and SiC.

Molecular beam epitaxy (MBE)

- Theoretical principles.

- Applications to the growth of epitaxial films.

Chemical Beam Epitaxy

- Theoretical principles and applications.

Sol-gel deposition techniques

Theoretical principles.

- Applications to film synthesis, hybrid systems, nanoparticles by Stober process.

Precursors for vapor phase and solution processes

Synthesis of nano structured materials

- Definition of nanostructures.

- Synthetic approaches for the synthesis of nanostructures.

- Nanorod synthesis and vapor phase nanotubes.

- Synthesis of nanoparticles and solution nanostructures

Monolayer synthesis

Molecular layer deposition for the deposition of monolayers.

Notes on the synthesis of self-assembled monolayer from solution.

 

TYPES OF MATERIALS

- Perovskite structure

- Structure description and tolerance factor

Structure-property relationship

- Perovskites with ionic conduction properties

- Description of ionic conductivity of intrinsic and extrinsic type.

- Solid oxide fuel cells.

Perovskites with dielectric properties

- Piezoelectric, pyroelectric and ferroelectric.

- Applications in energy harvester.

- Notes on piezotronic, piezophotonic and piezo-phototronic

Perovskite-based materials with superconducting properties

- Basic and superconducting principles I and II type. -

- Outline of BCS theory.

- Case studies of systems based on high Tc superconductors

 

CHARACTERIZATION METHODOLOGIES

X-ray production.

- Information obtainable from a diffractogram: amorphous or crystalline nature, phase identification, grain size.

- Crystalline lattices and systematic absences.

- Diffractions from powders and thin films: calculation of cell parameters.

- Notes on the single crystal: Ewald sphere.

- Advanced characterization of materials: rocking curves and polar figures in the characterization of oriented and epitaxial samples

 

Electronic scanning microscopy

- General principles.

- Tungsten filament electron beam, LaB6 crystal, or FEG (Field Emission Gun).

- Volume of interaction, elastic and inelastic events, species produced.

- Detector of secondary and backscattered electrons.

 

EDX Microanalysis (Energy Dispersive X-ray Analysis)

- Detector type

- Qualitative and quantitative analysis (ZAF method).

- Maps and scan-lines via EDX.

 

WDX (Wavelength Dispersive X-ray Analysis) microanalysis

- Spectrometer and crystal type description

- Qualitative and quantitative analysis.

- Advantages and disadvantages of the two microanalysis

Textbook Information

1)  A. R. West “Basic Solid State Chemistry and its Applications” Wiley, 2012;  

2)  B. D. Fahlman “Materials Chemistry” 3rd Edition, Springer, 2018; 

3) Editor R.  Fisher, "Precursor Chemistry of Advanced Materials: CVD, ALD and Nanoparticles", Springer, 2010.

4) L. V. Interrante e M. J. Hampden-Smith Chemistry of Advanced Materials Wiley-VCH, 1998.  

Lecture handouts.

Course Planning

 SubjectsText References
1Temporal ALD and Spatial ALD Case studies: deposition of simple oxides (Al2O3); synthesis of photonic crystals; deposition of multicomponent systems.Handouts
2Chemical Vapor Deposition (CVD) and Metal-Organic-CVD: basics and applicationsHandouts
3Molecular beam epitaxy (MBE). Handouts
4Chemical Beam Epitaxy: basics and applicationsHandouts
5Sol-gel deposition. Precursors for sol.-gel. Applications.Handouts
6Precursors for vaor phase  and solution processesHandouts
7Perovskites: structure and tolerance factorHandouts
8Ionic conductors. Solid oxide fuel cells.Handouts
9Dielectric materials: Piezo-, piro- and ferroelectric materials.Handouts
10Hgt Tc superconductorsHandouts
11X-ray diffractionWest and Fahlam, Handouts
12Characterization of oriented and epitaxial samples: rocking curves and pole figures.Handouts
13Scanning electron microscopy: General principles. Interaction volume, elastic and inelastic events, produced species. Detectors of secondary electrons and backscattered electrons.Handouts
14 EDX Microanalysis (Energy Dispersive X-ray Analysis) and WDX (Wavelength Dispersive X-ray Analysis):  qualitative and quantitative analyses. Advantages and disadvantages of the two techniquesHandouts

Learning Assessment

Learning Assessment Procedures

Oral exams.

Learning assessment may also be conducted electronically, if circumstances require it.

Examples of frequently asked questions and / or exercises

Typical Questions:

- Thin Film Synthesis Techniques.

- Atomic Layer Deposition.

- Molecular Beam Epitaxy: Applications and Advantages.

- Sol-Gel: Applications to the Synthesis of Materials in Various Forms.

- Ionic Conductivity and SOFCs.

- Vapor-Phase Nanostructures.

- Dielectric Materials: Properties and Applications.

- Ferroelectric Materials.

- X-ray Diffraction: Phase Analysis, Rocking Curves, and Pole Figures.

- Morphological Characterization of Materials: Scanning Electron Microscopy.

- Energy- and Wavelength-Dispersive X-ray Microanalysis.