Synthesis methodologies

Precise control of the materials properties implies mastering the atomic-, nano-, meso- and macro-scales. In the case of nanoparticles, this means tunability of the crystal structure, the particle size and morphology, and ability to process them as a large ensemble to form the final material. We are exploring new ways to synthesize and process nano-objects that cannot be obtained by usual methods. We especially aim at developing more sustainable routes: Soft chemistry (« Chimie douce ») in water , colloidal synthesis in molten salts, and combination of the sol-gel process with carbothermal reduction.

Overviews of our approaches

  1. Geoinspired syntheses of materials and nanomaterials, D. Portehault*, I. Gómez-Recio, M. A. Baron, V. Musumeci, C. Aymonier, V. Rouchon, Y. Le Godec, Chemical Society Reviews, 51, 4828 (2022)
  2. Beyond the compositional threshold of nanoparticle-based materials, D. Portehault*, S. Delacroix, G. Gouget, R. Grosjean, T.-H.-C. Chan-Chang, Accounts of Chemical Research, 51, 930–939 (2018)

Syntheses in molten salts

  1. Transforming Nanocrystals into Superhard Boron Carbide Nanostructures, F. Igoa Saldaña, T. Gaudisson, S. Le Floch, B. Baptiste, L. Delbes, V. Malarewicz, O. Beyssac, K. Béneut, C. Coelho Diogo, C. Gervais, G. Rousse, K. Rasim, Y. Grin, A. Maître, Y. Le Godec*, D. Portehault*, ACS Nano,  18, 30473 (2024)
  2. Covalent Transition Metal Borosilicides: Reaction Pathways in Molten Salts for Water Oxidation Electrocatalysis, D. Janisch, F. Igoa Saldaña, E. De Rolland Dalon, C. VM Inocêncio, Y. Song, P.-O. Autran, A. Miche, S. Casale, D. Portehault*, Journal of the American Chemical Society,  146, 21824 (2024)
  3. Galvanic Replacement and Etching of MAX-Related Phases in Molten Salts toward MXenes: An In Situ Study, E. Defoy, M. Baron, A. Séné, A. Ghoridi, D. Thiaudière, S. Célérier, P. Chartier, F. Brette, V. Mauchamp, D. Portehault*, Chemistry of Materials, 35, 19, 8112–8121 (2023)
  4. Heterostructured Cobalt Silicide Nanocrystals: Synthesis in Molten Salts, Ferromagnetism, and Electrocatalysis, Y. Song, I. Gómez-Recio, A. Ghoridi, F. Igoa Saldaña, D. Janisch, C. Sassoye, V. Dupuis, D. Hrabovsky, M. L. Ruiz-González, J. M. González-Calbet, S. Casale, A. Zitolo, B. Lassalle-Kaiser, C. Laberty-Robert, D. Portehault*, Journal of the American Chemical Society, 145, 19207 (2023)
  5. Molten Salts‐Driven Discovery of a Polar Mixed‐Anion 3D Framework at the Nanoscale: Zn4Si2O7Cl2, Charge Transport and Photoelectrocatalytic Water Splitting, R. Kumar, Y. Song, A. Ghoridi, P. Boullay, G. Rousse, C. Gervais, C. Coelho Diogo, H. Kabbour, C.  Sassoye, P. Beaunier, V. Castaing, B. Viana, M. L. Ruiz Gonzalez, J. Gonzalez Calbet, C. Laberty‐Robert, D. Portehault*, Angewandte Chemie International Edition, 135, e202303487 (2023)
  6. Tuning of Oxygen Electrocatalysis in Perovskite Oxide Nanoparticles by the Cationic Composition, M. Han, I. Gómez-Recio, D. Gutiérrez Martín, N. Ortiz Peña, M. L. Ruiz-González, M. Selmane, J. M. González-Calbet, O. Ersen, A. Zitolo, B. Lassalle-Kaiser*, D. Portehault*, C. Laberty-Robert*, ACS Catalysis, 13, 8, 5733–5743 (2023)
  7. Revealing the Elusive Structure and Reactivity of Iron Boride α-FeB, F. Igoa Saldaña, E. Defoy, D. Janisch, G. Rousse, P.-O. Autran, A. Ghoridi, A. Séné, M. Baron, L. Suescun, Y. Le Godec, D. Portehault*, Inorganic Chemistry, 62, 2073 (2023)
  8. Converting silicon nanoparticles into nickel iron silicide nanocrystals within molten salts for water oxidation electrocatalysis, Y. Song, S. Casale, A. Miche, D. Montero, C. Laberty-Robert, D. Portehault, Journal of Materials Chemistry A, 10, 1350 (2022)
  9. Electron Precise Sodium Carbaboride Nanocrystals from Molten Salts: Single Sources to Boron Carbides, S. Delacroix, F. Igoa, Y. Song, Y. Le Godec, C. Coelho-Diogo, C.  Gervais, G. Rousse, D. Portehault*, Inorganic Chemistry, 60,  4252 (2021)
  10. Phase selective synthesis of nickel silicide nanocrystals in molten salts for electrocatalysis of the oxygen evolution reaction, R. Kumar, M. Bahri, Y. Song, F. Gonell, C. Thomas, O. Ersen, C. Sanchez, C. Laberty-Robert, D. Portehault*, Nanoscale, 12, 15209 (2020)
  11. Structure-activity relationship in manganese perovskite oxide nanocrystals from molten salts for efficient oxygen reduction reaction electrocatalysis, F. Gonell, C. M. Sanchez-Sanchez, V. Vivier, C. Méthivier, C. Laberty-Robert, D. Portehault*, Chemistry of Materials, 32, 4241 (2020)
  12. Multicationic Sr4Mn3O10 mesostructures: molten salt synthesis, analytical electron microscopy study and reactivity, I. N. González-Jiménez, A. Torres-Pardo, S. Rano, C. Laberty-Robert, J. C. Hernández-Garrido, M. López-Haro, J. J. Calvino, Á. Varela, C. Sanchez, M. Parras,* J. M. González-Calbet, D. Portehault*, Materials Horizons, 5, 480-485 (2018)
  13. Surface-driven magnetotransport in perovskite nanocrystals, H. L. Thi N’Goc, D. Notemgnou Mouafo, C. Etrillard, A. Torres-Pardo, J.-F. Dayen, S. Rano, G. Rousse, C. Laberty-Robert, J. Gonzales Calbet, M. Drillon, C. Sanchez, B. Doudin, D. Portehault*, Advanced Materials, 10.1002/adma.201604745 (2017)
  14. New route toward nanosized crystalline metal borides with tuneable stoichiometry and variable morphologies, G. Gouget, P. Beaunier, D. Portehault*, C. Sanchez*, Faraday Discussions, 191, 511 (2016) Invited article
  15. A general solution route toward metal boride nanocrystals, D. Portehault,* S. Devi, P. Beaunier, C. Gervais, C. Giordano, C. Sanchez, M. Antonietti, Angewandte Chemie, International Edition, 50, 3262, (2011) Inside cover article, communication VIP.
  16. Boron carbon nitride nanostructures from salt melts: tunable water-soluble phosphors, W. Lei, D. Portehault,* R. Dimova, M. Antonietti, Journal of the American Chemical Society, 133, 7121, (2011)

Precipitation in water

  1. Metal–Support Interactions in Pt-WO3 Heterostructures: Role of WO3 Polymorphism, I. Gómez-Recio, C. Thomas, C. Méthivier, M. L. Ruiz-González, J. M. González-Calbet*, D. Portehault*, Chemistry of Materials, 35, 19, 7931–7942 (2023)
  2. Exceptional Low-Temperature CO Oxidation over Noble-Metal-Free Iron-Doped Hollandites: An In-Depth Analysis of the Influence of the Defect Structure on Catalytic Performance, I. Gómez-Recio, H. Pan, A. Azor-Lafarga, M. L. Ruiz-González, M. Hernando, M. Parras, M. T. Fernández-Díaz, J. J. Delgado, X. Chen, D. Goma Jiménez, D. Portehault, C. Sanchez, M. Cabero, A. Martínez-Arias, J. M. González-Calbet*, J. J. Calvino*, ACS Catalysis, 11, 15026 (2021)
  3. Structure and electrochromism of two-dimensional octahedral molecular sieve h’-WO3, J. Besnardiere, B. Ma, A. Torres-Pardo, G. Wallez, H. Kabbour, J. M. González-Calbet, H. J. Von Bardeleben, B. Fleury, V. Buissette, C. Sanchez, T. Le Mercier, S. Cassaignon, D. Portehault*, Nature Communications, 10, 327 (2019)
  4. Nanoparticles of Low-Valence Vanadium Oxyhydroxides: Reaction Mechanisms and Polymorphism Control by Low-Temperature Aqueous Chemistry, J. Besnardiere, X. Petrissans, F. Ribot, V. Briois, C. Surcin, M. Morcrette, V. Buissette, T. Le Mercier, S. Cassaignon, D. Portehault*, Inorganic Chemistry, 55, 11502 (2016)
  5. One step microwave-assisted synthesis of nanocrystalline WOx–ZrO2 acid catalysts, F. Gonell, D. Portehault, B. Julián-López, K. Vallé, C. Sanchez, A. Corma, Catalysis Science & Technology, 6, 8257 (2016)
  6. New Synthesis Strategies of Luminescent YVO4:Eu Nanoparticles with H2O2 Selective Sensing Properties, N. Duée, C. Ambard, F. Pereira, D. Portehault, B. Viana, K. Valle, D. Autissier, C. Sanchez, Chemistry of Materials, 27, 5198 (2015)
  7. Evolution of nanostructured manganese (oxyhydr)oxides in water through MnO4- reduction, D. Portehault, S. Cassaignon, E. Baudrin, J. P. Jolivet, Crystal Growth & Design, 10, 2168, (2010)
  8. Structural and morphological control of manganese oxide nanoparticles upon soft aqueous precipitation through MnO4-/Mn2+ reaction, D. Portehault, S. Cassaignon, E. Baudrin, J. P. Jolivet, Journal of Materials Chemistry, 19, 2407, (2009)

Syntheses in hydrofluxes

  1. Crystallization of Manganese(V) Oxides by Hydroflux Synthesis: Control of Anisotropic Growth and Electrochemical Stability, C. V. M. Inocêncio, A. Torres-Pardo, D. Montero, L. Roach, P.-O. Autran, C. Sassoye, C. Aymonier, A. Varela, M. Parras, C. Laberty-Robert, D. Portehault*, Inorganic Chemistry, 10.1021/acs.inorgchem.4c05439

Microwave-assisted synthesis

  1. One step microwave-assisted synthesis of nanocrystalline WOx–ZrO2 acid catalysts, F. Gonell, D. Portehault, B. Julián-López, K. Vallé, C. Sanchez, A. Corma, Catalysis Science & Technology, 6, 8257 (2016)
  2. New Synthesis Strategies of Luminescent YVO4:Eu Nanoparticles with H2O2 Selective Sensing Properties, N. Duée, C. Ambard, F. Pereira, D. Portehault, B. Viana, K. Valle, D. Autissier, C. Sanchez, Chemistry of Materials, 27, 5198 (2015)

Combination of the sol-gel process and carbothermal reduction

  1. Original Electrospun Core-Shell Nanostructured Magnéli Titanium Oxide Fibers and their Electrical Properties, V. Maneeratana, D. Portehault,* J. Chaste, D. Mailly, M. Antonietti, C. Sanchez, Advanced Materials, 26, 2654 (2014)
  2. Facile general route toward tunable Magneli nanostructures and their use as thermoelectric metal oxide/carbon nanocomposites, D. Portehault,* V. Maneeratana, C. Candolfi, N. Oeschler, I. Veremchuk, Y. Grin, C. Sanchez, M. Antonietti, ACS Nano, 5, 9052, (2011)

Investigation of reaction mechanisms

  1. Covalent Transition Metal Borosilicides: Reaction Pathways in Molten Salts for Water Oxidation Electrocatalysis, D. Janisch, F. Igoa Saldaña, E. De Rolland Dalon, C. VM Inocêncio, Y. Song, P.-O. Autran, A. Miche, S. Casale, D. Portehault, Journal of the American Chemical Society,  146, 21824 (2024)
  2. Galvanic Replacement and Etching of MAX-Related Phases in Molten Salts toward MXenes: An In Situ Study, E. Defoy, M. Baron, A. Séné, A. Ghoridi, D. Thiaudière, S. Célérier, P. Chartier, F. Brette, V. Mauchamp, D. Portehault*, Chemistry of Materials, 35, 19, 8112–8121 (2023)
  3. In situ liquid transmission electron microscopy reveals self-assembly-driven nucleation in radiolytic synthesis of iron oxide nanoparticles in organic media, N. Ortiz Peña, D. Ihiawakrim, S. Creţu, G. Cotin, C. Kiefer, S. Begin-Colin, C. Sanchez, D. Portehault, O. Ersen, Nanoscale, 14, 10950 (2022)
  4. A Confinement‐Driven Nucleation Mechanism of Metal Oxide Nanoparticles Obtained via Thermal Decomposition in Organic Media, G. Cotin, B. Heinrich, F. Perton, C. Kiefer, G. Francius, D. Mertz, B. Freis, B. Pichon, J.‐M. Strub, S. Cianférani, N. Ortiz Peña, D. Ihiawakrim, D. Portehault, O. Ersen, A. Khammari, M. Picher, F. Banhart, C. Sanchez, S. Begin‐Colin, Small, 18, 2200414 (2022)
  5. Experimental Descriptors for the Synthesis of Multicationic Nickel Perovskite Nanoparticles for Oxygen Reduction, F. Gonell, C. M. Sanchez Sanchez, V. Vivier, C. Laberty-Robert, D. Portehault*, ACS Applied Nanomaterials, 3, 7482 (2020)
  6. Nanoparticles of Low-Valence Vanadium Oxyhydroxides: Reaction Mechanisms and Polymorphism Control by Low-Temperature Aqueous Chemistry, J. Besnardiere, X. Petrissans, F. Ribot, V. Briois, C. Surcin, M. Morcrette, V. Buissette, T. Le Mercier, S. Cassaignon, D. Portehault*, Inorganic Chemistry, 55, 11502 (2016)
  7. The core contribution of transmission electron microscopy to functional nanomaterials engineering, S. Carenco, S. Moldovan, L. Roiban, I. Florea, D Portehault, K. Vallé, P. Belleville, C. Boissière, L. Rozes, N. Mézailles, M. Drillon, C. Sanchez, O. Ersen, Nanoscale, 8, 1260 (2016)
  8. A general solution route toward metal boride nanocrystals, D. Portehault,* S. Devi, P. Beaunier, C. Gervais, C. Giordano, C. Sanchez, M. Antonietti, Angewandte Chemie, International Edition, 50, 3262, (2011) Inside cover article, communication VIP.
  9. Evolution of nanostructured manganese (oxyhydr)oxides in water through MnO4- reduction, D. Portehault, S. Cassaignon, E. Baudrin, J. P. Jolivet, Crystal Growth & Design, 10, 2168, (2010)
  10. Structural and morphological control of manganese oxide nanoparticles upon soft aqueous precipitation through MnO4-/Mn2+ reaction, D. Portehault, S. Cassaignon, E. Baudrin, J. P. Jolivet, Journal of Materials Chemistry, 19, 2407, (2009)