Study-unit ADVANCED CHARACTERIZATION OF INORGANIC MATERIALS
| Course name | Chemical sciences |
|---|---|
| Study-unit Code | A001111 |
| Curriculum | Comune a tutti i curricula |
| Lecturer | Ferdinando Costantino |
| Lecturers |
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| Hours |
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| CFU | 6 |
| Course Regulation | Coorte 2023 |
| Supplied | 2024/25 |
| Supplied other course regulation | |
| Learning activities | Affine/integrativa |
| Area | Attività formative affini o integrative |
| Sector | CHIM/03 |
| Type of study-unit | Opzionale (Optional) |
| Type of learning activities | Attività formativa monodisciplinare |
| Language of instruction | Italian |
| Contents | The course of advanced characterization of inorganic materials is divided into two parts: in the first part the chemical and structural aspects of ionic, molecular and covalent solids will be studied with particular emphasis on crystallography and symmetry of crystalline solids. In the second part, some of the main solid state characterization techniques will be treated in order to obtain structural information and to describe the main properties of the materials studied. In particular, the course will focus on: X-ray diffraction, X-ray absorption and emission spectroscopies, electronic microscopies, thermal analysis, surface area analysis and ICP chemical composition. The course provides practical use of the instruments available at the department. |
| Reference texts | -J. C. Vickerman, S. Gilmor. Surface Analysis. The principle techniques Second Edition. Wiley Ltd. Publications. -L.E. Smart. Solid State Chemistry, An introduction. Fourth Edition CRC Press |
| Educational objectives | The course aims to provide an adequate knowledge of the characteristics of inorganic solids from a chemical and structural point of view. The crystallographic aspects of Ionic solids and the electronic structure of covalent solids will be investigated for this purpose. The student will be provided then an overview of the main investigation techniques currently used in materials chemistry. The student must be able, at the end of the course, to choose the appropriate characterization techniques and know how to interpret the results in order to completely describe an inorganic material being studied. |
| Prerequisites | The basic prerequisites to follow the course profitably are an adequate preparation in inorganic chemistry and solid state. An adequate knowledge of mathematics and physics of electromagnetic systems is also required. I also recommend the frequency of the "chemistry of inorganic materials" course |
| Teaching methods | Frontal lessons integrated to several laboratory experiences in the second part of the course. |
| Other information | In each of the exam periods planned according to the calendar of teaching activities, at least a couple of dates are scheduled for the exam. Students are required to register for the exam following the University procedure. In case of problems and difficulties students are invited to contact the teachers. The student can participate in all the required exam tests. |
| Learning verification modality | The examination will consist in an oral test on the topics explained during the course. Moreover, during the oral test, the student will be asked to describe qualitatively the experimental data acquired on a material under investigation in order to determine its chemical composition and the main properties. |
| Extended program | States of aggregation of matter. Amorphous state and crystalline state. Elements of morphologic crystallography. Points, rows and planes. Elementary cells in 2 and 3D. I and II laws of morphological crystallography. Symmetry point operations. Symmetry operators of I and II species. Rotations, inversions and translations. The 32 point classes. The 7 crystalline systems. Bravais lattices. Space groups. Reading and understanding the international tables of crystallography. Ionic solids. Ionic interactions. Reticular Energy. Madelung constant. Repulsive interactions. Born Landè equation. Kaputinsky equation. Thermal stability of ionic solids. Born Haber cycle. Ionic radiis. Univalent and crystalline radiis. Coordination number. Pauling's laws. Stability of ionic solids. Compact packings. Cubic and hexagonal packings. Centered lattices. Calculation of the atomic packing factor. Planar and linear density. Theoretical density calculation. Trigonal, octahedral and tetrahedral cavities. Geometric calculations. Structures type of ionic solids: Blenda, Zinc-Blenda, fluorite, Antifluorite, NaCl, CsCl, Perovskite, rutile and Anatase. Notes on defects and dislocations in crystals. Covalent solids. Notes on the covalent bond. Band structures of metal solids, semiconductors and insulators. Band structures of inorganic solids. X-ray diffraction. X-Ray generation. Laboratory sources and unconventional. Synchrotron light. Brightness of the photons. X-ray interaction with matter. Thomson and Compton Scattering. Absorption. Fluorescence. Electron Scattering. Atomic Scattering. Scattering factor. Elementary cell Scattering. Reciprocal lattice. Laws of Laue. Bragg's law. Electronic density. Structure factor. Phase problem. Phase problem resolution methods. Direct methods and Patterson's function. Single crystal Diffraction: Geometries with 3 and 4 circles. X-ray detectors. Orientation Matrix. Data collection strategies. Integrated intensities and calculation of F2. Factors of agreement. Powder diffraction: Bragg Brentano and Debye Scherrer geometries. Instrumental aberrations. Instrumental and intrinsic profile of the sample. Contribution of size-strain. Profile functions. Notes on the methods of resolution AB-initio and refining Rietveld. The crystallographic file and its information. An overview of atomic force microscopy. X-ray absorption spectroscopies. EXAFS and XANES spectroscopies. Radial distribution functions. Photoelectron emission spectroscopies (XPS) Thermogravimetry. Differential thermal analysis. Differential scanning calorimetry. Surface area measurements. Micro-, meso-and macro-porosity. Pore distribution. Absorption isotherm of N2. Langmuir theory. BET theory. Physis-and Chemi-sorption. Isosteric heat. CO2 absorption. Notes on ICP-NOE analysis. Practical Exercises on the characterization fo porous organometallic solids. |