Functionalized Inorganic Fluorides : Synthesis, Characterization and Properties of Nanostructured Solids

Alain Tressaud






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Functionalized Inorganic Fluorides: Synthesis, Characterization & Properties of Nanostructured Solids covers several classes of nanostructured and functionalized inorganic fluorides, oxide-fluorides, and fluorinated oxides such as silica and alumina. Ranging from powders or glass-ceramics to thin layers and coatings, they have applications as more efficient and less aggressive catalysts, UV absorbers, planar optical waveguides, integrated lasers and optical amplifiers, luminescent materials, anti-reflective coatings and high Tc superconductors.

With a focus on new types of solids, such as nanopowders, hybrids, mesoporous fluorides, and intercalation compounds, the book covers new synthesis routes; physical-chemical characterizations - including morphology, structure, spectroscopic and optical behaviour; detailed ab initio investigations and simulations; and -last but not least- potential applications.


List of Contributors.

1 Sol-Gel Synthesis of Nano-Scaled Metal Fluorides – Mechanism and Properties (Erhard Kemnitz, Gudrun Scholz, Stephan Rüdiger).

1.1 Introduction.

1.2 Fluorolytic Sol-Gel Synthesis.


2 Microwave-Assisted Route Towards Fluorinated Nanomaterials (Damien Dambournet, Alain Demourgues and Alain Tressaud).

2.1 Introduction.

2.2 Introduction to Microwave Synthesis.

2.3 Preparation of Nanosized Metal Fluorides.

2.4 Concluding Remarks.



3 High Surface Area Metal Fluorides as Catalysts (Erhard Kemnitz and Stephan Rüdiger).

3.1 Introduction.

3.2 High Surface Area Aluminium Fluoride as Catalyst.

3.3 Host-Guest Metal Fluoride Systems.

3.4 Hydroxy(oxo)fluorides as Bi-acidic Catalysts.

3.5 Oxidation Catalysis.

3.6 Metal Fluoride Supported Noble Metal Catalysts.


4 Investigation of Surface Acidity using a Range of Probe Molecules (Alexandre Vimont, Marco Daturi and John M. Winfield).

4.1 Introduction.

4.2 Characterisation of Acidity on a Surface: Contrasts with Molecular Fluorides.

4.3 Experimental Methodology.

4.4 Experimental Studies of Surface Acidity.

4.5 Conclusions.


5 Probing Short and Medium Range Order in Al-based Fluorides using High Resolution Solid State Nuclear Magnetic Resonance and Parameter Modelling (Christophe Legein, Monique Body, Jean-Yves Buzaré, Charlotte Martineau and Gilles Silly).

5.1 Introduction.

5.2 High Resolution NMR Techniques.

5.3 Application to Functionalized Al-Based Fluorides with Catalytic Properties.

5.4 Alkali and Alkaline-earth Fluoroaluminates: Model Compounds for Modelling of NMR Parameters.

5.5 Conclusion.


6 Predictive Modelling of Aluminium Fluoride Surfaces (Christine. L. Bailey, Sanghamitra Mukhopadhyay, Adrian Wander, Barry Searle and Nicholas Harrison).

6.1 Introduction.

6.2 Methodology.

6.3 Geometric Structure of α and β-AIF3.

6.4 Characterization of AlF3 Surfaces.

6.5 Surface Composition under Reaction Conditions.

6.6 Characterization of Hydroxylated Surfaces.

6.7 Surface Catalysis.

6.8 Conclusions.



7 Inorganic Fluoride Materials from Solvay-Fluor and their Industrial Applications (Placido Garcia Juan, Hans-Walter Swidersky, Thomas Schwarze and Johannes Eicher).

7.1 Introduction.

7.2 Hydrogen Fluoride.

7.3 Elemental Fluorine, F2.

7.4 Iodine Pentafluoride, IF5.

7.5 Sulfur Hexafluoride, SF6.

7.6 Ammonium Bifluoride, NH4HF2.

7.7 Potassium Fluorometalates, KZnF3 and K2SiF6.

7.8 Cryolite and Related Hexafluoroaluminates, Na3AlF6, Li3AlF6, K3AlF6.

7.9 Potassium Fluoroborate, KBF4.

7.10 Fluoboric Acid, HBF4.

7.11 Barium Fluoride, BaF2.

7.12 Synthetic Calcium Fluoride, CaF2.

7.13 Sodium Fluoride, NaF.

7.14 Sodium Bifluoride, NaHF2.

7.15 Potassium Bifluoride, KHF2.

7.16 Potassium Fluoroaluminate, KAlF4.

7.17 Fluoroaluminate Fluxes in Aluminum Brazing.

7.18 Summary.


8 New Nanostructured Fluorocompounds as UV Absorbers (Alain Demourgues, Laetitia Sronek and Nicolas Penin).

8.1 Introduction.

8.2 Synthesis of Tetravalent Ce and Ti-based Oxyfluorides.

8.3 Chemical Compositions and Structural Features of Ce and Ti-based Oxyfluorides:.

8.4 UV Shielding Properties of Divided Oxyfluorides.

8.5 Conclusion.



9 Oxyfluoride Transparent Glass Ceramics (Michel Mortier and Géraldine Dantelle).

9.1 Introduction.

9.2 Synthesis.

9.3 Different Systems.

9.4 Thermal Characterization.

9.5 Morphology of the Separated Phases.

9.6 Optical Properties of Glass-Ceramics.

9.7 Conclusion.


10 Sol-Gel Route to Inorganic Fluoride Nanomaterials with Optical Properties (Shinobu Fujihara).

10.1 Introduction.

10.2 Principle of a Sol-Gel Method.

10.3 Fluorinating Reagents and Method of Fluorination.

10.4 Control of Shapes and Microstructures.

10.5 Optical Properties.

10.6 Concluding Remarks.


11 Fluoride Glasses and Planar Optical Waveguides (Brigitte Boulard).

11.1 Introduction.

11.2 Rare Earth in Fluoride Glasses.

11.3 Fabrication of Waveguides: A Review.

11.4 Performances of Active Waveguides.

11.5 Fluoride Transparent Glass Ceramics: An Emerging Material.

11.6 Conclusion.


12 Polyanion Condensation in Inorganic and Hybrid Fluoroaluminates (Karim Adil, Amandine Cadiau, Annie Hemon-Ribaud, Marc Leblanc and Vincent Maisonneuve).

12.1 Introduction.

12.2 Synthesis.

12.3 Extended Finite Polyanions (0D).

12.4 1D Networks.

12.5 2D Networks.

12.6 3D Networks.

12.7 Evolution of the Condensation of Inorganic Polyanions.


Supplementary Materials.


13 Synthesis, Structure and Superconducting/Magnetic Properties of Cu- and Mn- Based Oxyfluorides (Evgeny V. Antipov and Artem M. Abakumov).

13.1 Introduction.

13.2 Chemical Aspects of Fluorination of Complex Oxides.

13.3 Structural Aspects of Fluorination of Complex Cuprates and Superconducting Properties.

13.4 Fluorination of Manganites.

13.5 Conclusions.


14 Doping Influence on the Defect Structure and Ionic Conductivity of Fluorine- containing Phases (Elena I. Ardashnikova, Vladimir A. Prituzhalovand I. B. Kutsenok).

14.1 Introduction.

14.2 Influence of Oxygen Ions on Fluoride Properties.

14.3 Cation Doping of Fluorides.

14.4 Active Lone Electron Pair of Cations and Ionic Conductivity.

14.5 Peculiarities of the Defect Structure of Nonstoichiometric Fluorite-like Phases.

14.6 Ionic Transfer in Fluorite-like Phases.

14.7 Peculiarities of the Defect Structure of Nonstoichiometric Tysonite-like Phases.

14.8 Ionic Transfer in Tysonite-like Phases.

14.9 Conclusions.


15 Hybrid Intercalation Compounds Containing Perfluoroalkyl Groups (Yoshiaki Matsuo).

15.1 Introduction.

15.2 Preparation and Properties of Intercalation Compounds Containing Perfluoroalkyl Groups.

15.3 Photophysical and Photochemical Properties of Dyes in Intercalation Compounds Containing Perfluoroalkyl Groups.

15.4 Conclusion and Future Perspectives.


16 The Fluoride Route: A Good Opportunity for the Preparation of 2D and 3D Inorganic Microporous Frameworks (Jean-Louis Paillaud, Philippe Caullet, Jocelyne Brendlé, Angélique Simon- Masseron and Joël Patarin).

16.1 Introduction.

16.2 Silica-based Microporous Materials.

16.3 Germanium-based Microporous Materials.

16.4 Phosphate-based Microporous Materials.

16.5 Synthetic Clays.

16.6 Conclusion.


17 Access to Highly Fluorinated Silica by Direct F2 Fluorination (Alain Demourgues, Emilie Lataste, Etienne Durand and Alain Tressaud).

17.1 Introduction.

17.2 Mesoporous Silica and Fluorination Procedures.

17.3 About the Chemical Composition and Morphology of Highly Fluorinated Silica.

17.4 FTIR Analysis.

17.5 Thermal Stability and Water Affinity of Highly Fluorinated Silica.

17.6 Nuclear Magnetic Resonance Investigations.

17.7 Conclusions on the F2-gas Fluorination Mechanism of Mesoporous Silica.



18 Preparation and Properties of Rare-earth Containing Oxide Fluoride Glasses (Susumu Yonezawa, Jae-ho Kim and Masayuki Takashima).

18.1 Introduction.

18.2 Preparation and Basic Characteristics of Oxide Fluoride Glasses Containing LnF3.

18.3 Optical and Magnetic Properties of LnF3-BaF2-AlF3-GeO2 (SiO2) Glasses.

18.4 Conclusion.


19 Switchable Hydrophobic-hydrophilic Fluorinated Layer for Offset Processing (Alain Tressaud, Christine Labrugère and Etienne Durand).

19.1 Introduction.

19.2 The Principles of Lithographic Printing Process.

19.3 Experimental Part.

19.4 Various Types of Surface Modifications using Fluorinated rf Plasmas.

19.5 Comparison of Surface Modifications of Porous Alumina using Various Fluorinated Media: CF4, C3F8 and c-C4F8.

19.6 Conclusion.




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