Description and contextualization of the subject

The subject "Modern techniques for the synthesis of nanomaterials (TU16)" is compulsory and is taught in the first quarter of the 2nd course of the Erasmus Mundus Master in Materials for Energy Storage and Conversion (MESCP+). This subject gives continuity to the obligatory subject of "Chemistry of Materials (TU2)" of the first semester of the 1st course of this Master, taught at the University of Warsaw (WUT, Poland), as well as to the obligatory subject of "State Chemistry" Advanced Solid (TU9) "of the second semester of the 1st year of this Master, taught at the University of Toulouse (UPS, France).

The subject will give an overview of various synthetic routes available for the preparation of materials with potential application in electrochemical energy storage (EES) systems. These materials can be employed as electrode materials (positive or negative) and / or electrolytes in systems such as batteries (Li-ion, Na-ion, metal-air, Li-sulfur, all solid batteries, etc.) and supercapacitors (EDLC, hybrid, etc). They include inorganic materials (oxides, polyanionic compounds, alloys, etc.), carbonaceous materials (porous carbons, graphite, graphene, carbon nanotubes and carbon derived from carbides, etc.) and polymeric materials (crystalline and amorphous polymers, mixtures of polymers, cross-linked polymers, block copolymers and polymeric compounds). Students will acquire basic knowledge about the variety of synthesis methods (eg. synthesis of solid-state, sol-gel, hydro- and solvo-thermal, by precipitation, pyrolysis, mechano-chemical, combustion, functionalization, activation, U-V crosslinking, grafting, solvent casting, etc.) at the disposition of the inorganic chemists to produce these different materials. They will also learn about the different parameters and variables of each type of synthesis that can influence the morphology and microstructure of the samples synthesized and, as a consequence, their physico-chemical and electrochemical properties.

Learning outcomes of the subject

- Know the main synthesis methods used for the production of inorganic, carbonaceous and polymeric materials used in electrochemical systems for energy storage (EES), and knows how to explain the main characteristics of these syntheses.



- Select a synthesis method (including possible precursors and experimental parameters) to produce a given inorganic, carbonaceous or polymeric material.



- Suggest alternatives to a synthesis or post-treatment of a sample to influence the morphology and microstructure of the synthesized samples, and consequently their physicochemical and electrochemical properties



- Perform basic synthesis tasks at the laboratory for the production of inorganic, carbonaceous and polymeric materials.



- Select proper characterization methods to control the purity of the synthesized sample.

Ordinary call: orientations and renunciation

The evaluation of the student will be made from the following tests and works:

1. A bibliography work on one of the topic of the course, prepared in a small group (between 2 and 4 students per group), and evaluated on a report written by the group and an oral presentation of the group (although the note of each student may vary according to the answers given by each student to the questions at the end of the oral presentation). The written report grade will contribute 20% to the final grade and the oral presentation grade will contribute 15% to the final grade.



2. An individual report presenting the preparation, the development and the results of laboratory work carried out by the students. This grade will contribute to 20% of the final grade.



3. A written individual exam, whose grade will contribute 20% to the final grade, and which will cover all the knowledge and competences addressed during the course (including lectures, laboratory work and literature work).



4. An individual oral examination, which will cover all the knowledge and competences addressed during the course (including lectures, laboratory work and literature work). This grade will contribute to 25% of the final grade.



The final grade will be calculated using the following formula:



Final grade = 0.20 (grade of the written report on the bibliography work) + 0.15 (grade of the presentation on the bibliography work) + 0.20 (grade of the laboratory practices) + 0.20 (grade of the individual written exam) + 0.25 (grade of the individual oral examination).



Students, to whom the above formula could be applied and who will obtain a grade equal to or higher than 5.0, will be approved.



Those students who have not carried out the activities to assess the learning outcomes throughout the course (bibliography work (1), laboratory practices (2)) should be examined of the corresponding competences through an additional oral exam.



Those students who do not attend the written final exams (3) and individual exams (4) will appear in the corresponding minutes as not presented.

Extraordinary call: orientations and renunciation

Students who are examined in the extraordinary call must complete the final written test being evaluated in it for the entire subject. That is, it is mandatory to solve the full written examination of the extraordinary call even if the partial exam has been approved.



For the calculation of the final grade, the same formula as in the ordinary call will be used. Those who can not apply the formula will also follow the procedure indicated in the ordinary call. Students who have not approved or have waived activities to evaluate the learning results throughout the course (laboratory practices, exercises, etc.) should be examined of the corresponding competences through an additional oral test in this extraordinary call.

Temary

1- Synthesis and processing of inorganic materials for EES systems

2- Synthesis and processing of polymeric materials for EES systems

3- Synthesis and processing of carbonaceous materials for EES systems

Bibliography

Compulsory materials

The students should use the collections of questions and problems that the professors will publish at the beginning of the course, and for each topic, on the eGela platform.







The student will have on the eGela platform, the syllabus of the subject and the scripts of practices in electronic format to promote understanding of the topics and the agile follow-up of the classes.

Basic bibliography

- Introduction to Computational Chemistry, 2nd Edition, WILEY, by F. Jensen.

- Computational Chemistry of Solid State Materials: A Guide for Materials Scientists, Chemists, Physicists and others, WILEY, by R. Dronskowski and R. Hoffmann

In-depth bibliography

- Modern Inorganic Synthetic Chemistry. ELSEVIER, by Xu and Xu.



- M.S. Whittingham (2009) Synthesis of Battery Materials. In: Nazri GA., Pistoia G. (eds) Lithium Batteries. Springer, Boston, MA. DOI: 10.1007/978-0-387-92675-9_3.



- V. Palomares, T. Rojo. (2012) Synthesis Processes for Li-Ion Battery Electrodes – From Solid State Reaction to Solvothermal Self-Assembly Methods. DOI: 10.5772/27496.



- Carbons for Electrochemical Energy Storage and Conversion Systems, Edited by Francois Beguin and Elzbieta Frackowiak, CRC Press (2009). ISBN 9781420053074



- Polymer electrolytes: fundamentals and application, César Sequeira, Diogo Santos, Woodhead Publishing in Materials, Elsevier, August 2010. ISBN 1845699777, 9781845699772.



- Solid Polymer Electrolytes: Fundamentals and Technological Applications, Fiona M. Gray, Wiley, 1991, ISBN: 0471187372, 9780471187370.



- Solid state ionics for batteries, T Minami , M. Tatsumigo, , M. Wakihara, C. Iwakura, , S. Kohjiya, I. Tanaka, Springer-Verlag, 2005, ISBN: 4-431-24974-5.

Journals

- Methods of synthesis and performance improvement of lithium iron phosphate for high rate Li-ion batteries: a review. T.V.S.L. Satyavani, A. Srivinas Kumar, P.S.V. Subba Rao. Engineering Science and Technology, an International Journal. 2015.



- From Charge Storage Mechanism to Performance: A Roadmap toward High Specific Energy Sodium‐Ion Batteries through Carbon Anode Optimization, Damien Saurel, Brahim Orayech, Biwei Xiao, Daniel Carriazo, Xiaolin Li, Teófilo Rojo, Advanced Energy Materials 8, 1703268 (2018)



- Polymer Electrolytes for Lithium-Based Batteries: Advances and Prospects, D. Zhou, D. Shanmukaraj, A. T. Kacheva, M. Armand. G. Wang, Chem 5, (2019) 2326.



- Production and processing of graphene and related materials, Claudia Backes et al. 2D Materials 7 (2020) 022001



- Three dimensional macroporous architectures and aerogels built of carbon nanotubes and/or graphene: synthesis and applications, Stefania Nardecchia, Daniel Carriazo, M. Luisa Ferrer, M. C. Gutierrez, Francisco del Monte, Chem. Soc. Rev., 42 (2013) 42, 794