Description and contextualization of the subject

This course, part of the third semester of the master's program, has a workload of 4.0 ECTS credits. During the second semester of the master's program at Université Toulouse III - Paul Sabatier, the course Advanced Solid State Chemistry is offered, covering, among other topics, crystal chemistry. The fundamental concepts of this discipline will be useful for the development of the present course.

In this course, students acquire the knowledge and skills necessary for the characterization of the crystalline structure of materials. Additionally, the study of surfaces that separate different phases of matter allows for a deeper understanding of how the properties and behaviours of these surfaces explain numerous phenomena related to the fabrication, processing, and applications of energy materials.

Learning outcomes of the subject

Knowledge or content:

RCO1: Knowledge of the physicochemistry of interfaces, especially solid surfaces, as well as surface characterisation techniques.

RCO2: Knowledge in the elucidation of the structure, properties and applications of different families of materials: metallic, polymeric, ceramic (including glasses), composites and functional materials.



Abilities or skills:

RHT1: Skills in diffraction data analysis and in determining structure using the Le Bail and Rietveld methods.

Ordinary call: orientations and renunciation

A) CONTINUOUS ASSESSMENT

The final grade for the course is divided as follows:

¿ Individual work: 45%

¿ Final exam: 55%

This applies to students who regularly attend classes (i.e., more than 75%) and actively participate in course activities.

Conditions / Restrictions:

Students must obtain a minimum score of 5 out of 10 in each of the components mentioned above.

No exceptions will be made regarding attendance or submission deadlines for students participating in the continuous assessment process.________________________________________

B) NON-CONTINUOUS ASSESSMENT

This applies to students who do not regularly attend classes (i.e., less than 75%) or to those who attend regularly but opt out of continuous assessment. The decision to opt out must be communicated to the course coordinator before the fourth week of classes.

In this case, assessment will be conducted through a Final Examination, which will evaluate all the learning outcomes established for the course.



Final Remarks:

1. The final written exam is mandatory for students who regularly attend classes but fail to achieve a minimum score of 5/10 in the continuous assessment.

2. If a student does not pass or does not participate in the Continuous Assessment process and does not take the Final Written Exam (whether through Continuous or Non-Continuous Assessment), they will receive a grade of EZ AURKEZTUA / NOT PRESENTED

Extraordinary call: orientations and renunciation

Students who do not pass in the regular exam session will be assessed through a Final Exam in the extraordinary exam session.

Temary

Thermodynamics of Solid Crystals

2. Review of Basic Concepts in Thermodynamics and Crystallization

Equilibrium and solubilities. Supersaturation. Seeding. Kinetics of crystallization processes. Primary and secondary crystallization.

3. Nucleation Theories

Homogeneous and heterogeneous nucleation. Classical theory. Advanced theories. Nucleation kinetics. Binary nucleation.

4. Solid Surfaces

Description of solid surfaces. Clean surfaces. Thermodynamics of solid surfaces. Solid-solid interfaces. Surface characterization techniques: microscopy, diffraction, and spectroscopy.

5. Surface Energy: Estimation and Application

Surface tension and changes in solubility. Experimental methods and contact angle measurement. Theories related to contact angle phenomena. Potential distortion model. Wetting. Water repellency. Flotation. Detergency.

6. Surface Area of Solids. Physisorption and Chemisorption

Surface area of solids. Structure and chemical nature of solid surfaces. Adsorption time. Langmuir adsorption isotherm. Experimental procedures. BET and related isotherms. Isotherms based on the equation of state of the adsorbed film. Comparison of surface areas using various multilayer models. Characteristic isotherm: related concepts. Physical adsorption: surface heterogeneity. Adsorption rate. Gas adsorption on porous solids: hysteresis.

7. Kinetics and Thermodynamics

Reaction rate and equations. Elementary vs. non-elementary reactions. Kinetics: reaction orders. Determination of rate law. Methods for determining reaction order.

8. Application to Heterogeneous Catalysis

Reaction mechanisms and rate-controlling step. Determination of the rate equation.

9. Introduction to X-ray Diffraction (XRD)

Simulation of an XRD pattern using FullProf. Extraction of integrated intensities using the Le Bail method (Profile Matching). Determination of the instrumental resolution function (IRF). Le Bail refinement using an IRF file to extract the apparent crystallite size. Rietveld refinement

Bibliography

Compulsory materials

Lecture notes provided by the teaching staff and accessible on the Egela platform.

Basic bibliography

- Mingos, M.P. (editor). The Periodic Table II - Catalytic, Materials, Biological and Medical Applications. Spinger (2019)

- Adamson, W. and Gast A.P. Physical Chemistry of Surfaces. 6th edition. Wiley-Interscience (1997).

- Butt, H.J., Graf, K. and Kappl, M. Physics and Chemistry of Interfaces. 2nd edition. Wiley-VCH (2006).

- McCash E.M. Surface Chemistry. Oxford University Press (2001).

- Eberhardt, J.P. Structural and Chemical Analysis of Materials. Wiley (1991)

- Bartholomew, C.H. and Farrauto C.J. Fundamentals of Industrial Catalytic Processes. 2ª edición. Wiley-Interscience (2006)

- Becher, P.; "Emulsions, theory and practice". Litton Educational Publishing Inc. (1972).

- Czichos, Saito, Smith (editors). Handbook of Metrology and Testing. Ed. Springer Verlag Berlin. 2nd Ed. (2011).

- Fogler, H.S., Elements of chemical reaction engineering, 4th Ed., Pearson-Prentice Hall, 2006.

- Young, R.A. The Rietveld Method. Reino Unido: International Union of Crystallography, 1993.

- International Tables for Crystallography, Volume A1: Symmetry Relations Between Space Groups. Alemania: Springer Netherlands, 2007.

In-depth bibliography

- Material-ES 2017 : 1 (4) ; paginas 63-82



- The hymalayan Physics, V. II, Contact Angle measuremnt for the surface Characterization of solids



- On Water repellency. DOI : 10.1039/b501657f



- Rao, K.H.; Forsberg, K.S.E.; "Interactions of anionic collectors in Flotation of semi-soluble salt minerals", in "Innovations in Flotation Technology".



- S.Lowell, J. E. Shields, M. A. Thomas and M. Thommes, Characterization of porous solids and powders: Surface area, pore size and density, Springer 2006.

Journals

-Chemical Engineering Abstracts.



-Chemical Engineering & Technology. Wiley-VCH, Weinheim.



-Chemie-Ingenieur Technik. Wiley-VCH, Weinheim.



-AlChE Journal. AIChE, New York.



-Ingeniería Química. Suplemento Nuevas Plantas. Ingeniería Química S.A., Madrid.



-Química e Industria. Asociación Nacional de Químicos de España, Madrid



-Chemical Engineering. McGraw-Hill, New York.



-Journal of Chemical Technology and Biotechnology. John Wiley and Sons, New York.

Links

http://www.acs.org



http://www.aiche.org



http://www.elsevier.com



http://www.accessscience.com



http://www.dekker.com



http://sciencedirect.com



https://www.ill.eu/sites/fullprof/



http://jp-minerals.org/vesta/en/