Unit INORGANIC MATERIALS: SYNTHETIS STRUCTURE AND PROPERTY

Course
Chemical sciences
Study-unit Code
A001115
Curriculum
Chimica inorganica per l'energia e la catalisi
Teacher
Ferdinando Costantino
Teachers
  • Ferdinando Costantino
Hours
  • 59 ore - Ferdinando Costantino
CFU
7
Course Regulation
Coorte 2022
Offered
2022/23
Learning activities
Caratterizzante
Area
Discipline chimiche inorganiche e chimico-fisiche
Academic discipline
CHIM/03
Type of study-unit
Obbligatorio (Required)
Type of learning activities
Attività formativa monodisciplinare
Language of instruction
Italian
Contents
Materials synthesis: sol-gel and solvothermal processes, precipitation and crystal growth, glass formation, chemical vapour deposition and aerosol processes. Reactivity of solids: solid-solid reactions, sintering, intercalation processes. Layered materials: clays, hydrotalcites and M(IV) phosphates and phosphonates. Micro-, meso- e macro-porous solids. MOFs. Polymer composites. Materials characterization techniques: thermal analysis, diffractometric studies, gas adsorption,optical measurements.
Reference texts
its applications", J. Wiley
U. Schubert, N. Hüsing, "Synthesis of Inorganic Materials", Wiley-VCH
Educational objectives
Main acquired knowledge

- Main features of the sol-gel process.
- Application of the sol-gel process to the fabrication of hybrid materials.
- Mechanisms of nucleation and crystal growth.
- Synthesis and crystal growth through solvothermal processes.
- Glass formation and main glass typologies.
Main skills
- To predict qualitatively the morphology of materials obtained through the sol-gel process.
- To predict the morphology of crystals formed form liquid phases (solutions or melts).
- To design the synthesis of hybrid materials through the sol-gel process.
- To design the synthesis of crystalline solids under hydrothermal conditions.
- To apply the chemical vapour transport in the purification of materials or in the growth of crystals.
- To assess the reactor type to be used in the formation of solids from the vapour phase.
- To use TGA and DSC techniques for the thermochemical characterization of materials.
- To use stress – strain tests for the mechanical characterization of materials.
- To assess qualitatively the mechanism of intercalation/ion-exchange processes through X-ray diffraction.
Prerequisites
You must have got a three-year degree in Chemical Sciences.
Teaching methods
The course consists in lectures (35 hours), and laboratory exercises (24 hours) focused on the preparation of polymer composites loaded with inorganic fillers and on their characterization by X-ray diffraction, TG analysis and stress - strain mechanical tests. Duplicated lecture notes edited by the teacher are available for some topics.
Other information
Lecture room: library of the Materials Chemistry Laboratory, Department of Chemistry, Biology and Biotechnology (buiding B).
Learning verification modality
The exam of the course consists in an oral interview of about half an hour on topics treated during the course (formation of solids from gas phase, from solutions and melts, reactivity of solids, layered solids, micro-, meso- and macro-porous solids, characterization techniques of materials). The first topic of the interview is chosen by the student. The test aims at ascertaining the knowledge level of the program topics and at testing the student communication skills and the his ability to process the acquired knowledge.
Extended program
REACTIVITY OF SOLIDS

Solid-solid reactions controlled by the diffusion of reagents. Solid-solid reactions controlled by the formation of nuclei. The sintering process.

Intercalation reactions. Intercalation in layered materials. Types of intercalation: direct intercalation, electrointercalation, intercalation of polymers, pillaring of layered compounds. Direct intercalation of Lewis basis in zirconium phosphate, alogens and metals in graphite, alkaline metals in metal transition disulfides. Graphene and carbon nanotubes. Electrointercalation in lithium batteries.
Polymer and oligomer intercalation.

Pillaring of layered compounds: Keggin-ion intercalation, pillared compounds arising from the functionalisation of the layers of zirconium phosphate; use of pillared compounds in the shape selective catalysis.

SELECTED CLASSES OF MATERIALS

Classification of silicates. Layered aluminosilicates: structural features, isomorphic replacement of Al(III) for Si(IV), of Mg(II) for Si(IV) and Li(I) for Mg(II). Clays: swelling and exfoliation.
Anionic clays.
Aluminosilicates with framework structure: feldspars and zeolites.
Zeolites: sodalitic cage, structural features, ion-exchange and catalytic properties as a function of the Si/Al molar ratio; use of zeolites in the shape selective catalysis.

Micro-, meso- and macro-porous solids.



Composite materials: micro- and nano-composites. Matrix – filler interactions. Synthetic approaches for the preparation of polymer composites.



PHYSICOCHEMICAL CHARACTERIZATION TECHNIQUES

Thermal analysis: thermogravimetric analysis, differential thermal analysis, differential scanning calorimerty.

Sress – strain mechanical tests: elastic, viscous and viscoelastic behaviour. Elastic modulus, yield strength, strength at break. Deformation mechanisms of amorphous polymers.

Determination of the surface area of solids by gas adsorption. Langmuir isotherm. BET model and BET isotherms. Types of adsorption isotherms. Hysteresis and capillary condensation.

Electrical conductivity measurements: elements of impedance spectroscopy.
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