The course aims to introduce students to the knowledge of structural chemistry of inorganic solids, binary phase diagrams and of the main experimental techniques for the structural (X-Ray Powder Diffraction), microstructural (Light Optical Microscopy, Scanning Electron Microscopy coupled with Electron Probe Microanalysis), calorimetric (Differential Scanning Calorimetry, Differential Thermal Analysis, Thermogravimetric Analysis) characterization of Inorganic Materials. The educational path is finalized to the development of the ability to judge by critical eye the experimental results.
The course includes lectures where the topics included in the programme will be explained and addressed and practice exercises which will be carried out in the classroom or at the research laboratory under the supervision of the teacher. An individual report at the end of the course concerning the practice exercises is requested.
The attendance of practice exercises is mandatory.
DiffractionTechniques. X-ray diffraction. Generation of X-rays. Crystal systems and and associated lattice parameters. Planes and Miller’s indices. Density of close packed structures. Tetrahedral and octahedral sites. Bravais lattices. Introduction to Symmetry Elements and Point Group Symmetry. Pearson’s symbols. Atomic positions within a crystal structure: description of some common structural prototypes. Crystal diffraction and Bragg’s Law. Debye-Scherrer method. Bragg-Brentano Powder diffractometer.
Microscopic Techniques. Conventional Optical Microscopy, Principle of Polarizing Microscope, bright field, dark field. Numerical aperture. Microscopic Resolution. Scanning Electron Microscopy (SEM). Configuration of SEM. Interaction of electron with samples. Secondary electrons. Backscattered electrons. Compositional and Topographic information. X-ray detectors: Energy Disperse X-ray Spectroscopy (EDS), Wavelenght-dispersive spectrometer (WDS).
Phase equilibria. Graphical representation. Liquid-solid binary systems. Non equilibrium freezing. Coring. Solid and interstitial solutions. Types of three-phase equilibria: eutectic, eutectoid, peritectic, peritectoid, monotectic, syntectic, catatectic. Some errors of construction. Scheil’s reaction scheme. Complex binary phase diagrams in inorganic chemistry.
Thermal and calorimetric techniques. Thermal analysis (TA) and differential thermal analysis (DTA). Differential scanning calorimetry (DSC): Heat Flow DSC, Power Compensation DSC, Calvet Calorimeter. Heat capacity measurements by using continuos mode or “step by step” mode in DSC and examples. Direct reaction Calorimetry for the enthalpy of formation measurements of solids. Thermogravimetric Analysis (TGA).
Training work: Lattice parameter determination by powder diffraction methods of metallic and NaxWO3 samples. Phase analysis using optical and electronic techniques. Interpretation of data obtained for binary alloys by DTA and DSC.
Structural Chemistry and Diffraction Methods
- Introduzione alla Chimica Moderna, M.Nardelli - Casa Editrice Ambrosiana,1978, p.41-45
- Diffrazione dei raggi X, H.P.Klug, L.E.Alexander, Alba Editrice, 1969, p. 1- 110 e 162-205
- Introduction to X-ray powder diffractometry, R.Jenkins, R.L.Snyder, Vol. 138 in Chemical Analysis a Series of monographs on Analytical Chemistry and Its Applications, J.D.Winefordner, series editor,1996, John Wiley &Sons, Inc.
Phase Diagrams
- "Phase Diagrams in Metallurgy", Rhines, Mc Graw-Hill Book Company, 1956, p. 1- 170
Thermoanalytical Techniques
- "Principi ed Applicazioni di calorimetria ed analisi termica", Ed. Piccin
- “Analisi Strumentale” H.E.Bauer, G.D.Christian, J.E.O’Reilly, Ed.Piccin, 1985
- Differential Thermal Analysis, M.I.Pope, M.D.Judd Heyden &Son 1977
- Calorimetry Fundamentals and Practice, W.Hemminger, G.Höhne, Verlag Chemie 1984
Ricevimento: By appointment.
SERENA DE NEGRI (President)
SIMONA DELSANTE (President)
NADIA PARODI (President)
GABRIELLA BORZONE
PAOLA RIANI
PAVLO SOLOKHA
Starting from September, 26, 2016, according to the timetable shown at www.ctc.unige.it
INORGANIC CHEMISTRY 2
The exam is oral, it is always conducted by two teachers and lasts approximately 60 minutes
The overall evaluation of the student includes the oral examination, the acquisition of practical skills considering the results obtained during the practice exercises and the quality of the individual reports.
The exams of the Inorganic Chemistry 1 with Laboratory and Principles of Mathematics Courses should be passed before.