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Preparation and characterization of metal nanoparticles supported on polymeric composites

VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali Perugia 12-15 Giugno 2007. Preparation and characterization of metal nanoparticles supported on polymeric composites. M. Sisani 1 , U. Costantino 1 , F. Costantino 1 , F. Presciutti 2 , A. Bottino 3 , G. Capannelli 3.

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Preparation and characterization of metal nanoparticles supported on polymeric composites

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  1. VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali Perugia 12-15 Giugno 2007 Preparation and characterization of metal nanoparticles supported on polymeric composites M. Sisani1, U. Costantino1, F. Costantino1, F. Presciutti2, A. Bottino3, G. Capannelli3 1Department of Chemistry, CEMIN, University of Perugia, Italy 2ISTM-CNR, SMAART, University of Perugia, Italy 3Department of Chemistry and Industrial Chemistry, University of Genova, Italy INSTM – Perugia 12-15 Giugno 2007

  2. Nanocomposites Nanometric particles dispersed into the organic matrix: 3 dimensions at nanometric scale 3Dparticles Spherical silica, nanoclusters of semiconductors etc. 2 dimensions at nanometric scale tubular structure Carbon nanotubes, nanowires etc. 1 dimension at nanometric scale lamellae Layered solids INSTM – Perugia 12-15 Giugno 2007

  3. The dispersion of a low loading (ca 5%) of inorganic particles of nanometric dimension into organic polymers allows the preparation of new composite materials with enhanced properties: • mechanical and thermal stability • gas barrier • flame retardant The presence of nanoparticles may induce new properties to the material: • electrical • optical • magnetic • biomedical • catalytic INSTM – Perugia 12-15 Giugno 2007

  4. Automotive gas tanks, bumpers, interior and exterior panels • Construction (building sections and structural panels) • Aerospace (flame retardant panels and high performance components) • Electrical and electronics (electrical components and printed circuit boards) • Food packaging (containers and wrapping films)

  5. Layered Inorganic ion exchangers posses unique properties to be active as filler of polymeric nanocomposites: • Exfoliation into single layers • Thickness of the layers at nanometric scale (about 1 nm) • High aspect ratio • Functionalization by ion exchange or grafting procedures of the layers increases the compatibility with the polymer and in some cases induces new properties for high-tech applications • Layered solids may intercalate polymeric chains into the interlayer region • Advantages of the incorporation of metal nanoparticles supported on polymeric composites: • Protect the metal nanoparticles from the oxidation • Control of the dimensions of the metal clusters • Very simple and effective method INSTM – Perugia 12-15 Giugno 2007

  6. Layered compounds dispersed in a polymeric matrix Layered microcrystal Polymer Nanocomposite: Lamellae dispersed in the polymer Nanocomposite: The polymer is intercalated In the interlamellar region Macrocomposite: two separate phases [1] [1] M. Alexandre, P. Dubois, Materals Science and Engineering (2000), 28, 1-63 INSTM – Perugia 12-15 Giugno 2007

  7. Chemical reduction Nanocomposite containing Cu metal nanoparticles Synthesis Polymeric matrix Polyvinylidene fluoride PVDF [2] Layered inorganic filler α-Zirconium PhosphateZr(HPO4)2 * H2Oconverted to ZrCu(PO4)2[3] [2] G. Alberti, M. Casciola et al., Solid State Ionics (2005), 176, 39 [3] G. Alberti, M. Casciola, U. Costantino, R. Vivani, Adv. Mat. (1996), 8, 291 INSTM – Perugia 12-15 Giugno 2007

  8. Gel di ZrCu(PO4)2 in DMF 1) Preparation of the colloidal dispersion of ZrCu(PO4)2 50% PrNH2 2) Exchange with Cu(CH3COO)2 Washing with DMF INSTM – Perugia 12-15 Giugno 2007

  9. PVDF/ ZrCu(PO4)2 Nanocomposite 2) Preparation of PVDF/ ZrCu(PO4)2 nanocomposite Intercalation from solution with DMF as solvent - Mixing - Stirring - Evaporation Solution of PVDF polymer in DMF Colloidal dispersion in DMF of ZrCu(PO4)2 INSTM – Perugia 12-15 Giugno 2007

  10. 1 cm 1 cm 3) Reduction and formation of metal nanoparticles S2O4= + Cu2+→ 2SO3= + Cu + 4H3O+ Pristine PVDF/ZrCu(PO4)2 nanocomposite PVDF/ZrPCu nanocomposite after chemical reduction with dithionite Several composites containing 2, 3, 5, 10, 15, 20 wt% of inorganic filler have been prepared and characterized by XRPD, UV-vis, AFM, HR-TEM techniques INSTM – Perugia 12-15 Giugno 2007

  11. XRPD patterns UV-vis Spectra INSTM – Perugia 12-15 Giugno 2007

  12. AFM images • PVDF polymer • PVDF/ZrCu(PO4)2 • PVDF/metal nanocomposite 5 wt% • PVDF/metal nanocomposite 10 wt% 3D AFM image of the surface of the reduced nanocomposite (5 wt%) INSTM – Perugia 12-15 Giugno 2007

  13. HR-TEM images a) PVDF polymer b) PVDF/ZrCu(PO4)2 10 wt% c) PVDF/ZrCu(PO4)2 20 wt% d) PVDF/metal nanocomposite 10 wt% e) PVDF/metal nanocomposite 10 wt% f) PVDF/metal nanocomposite 20 wt% INSTM – Perugia 12-15 Giugno 2007

  14. HR-TEM image of PVDF/metal nanocomposite 20 wt% after reduction and the magnification of a nanoparticle INSTM – Perugia 12-15 Giugno 2007

  15. Conclusion and further developments • This approach showed that multifunctional polymeric materials, with tunable chemical/physical properties, can be obtained by an easy and inexpensive synthesis • The use of a reducing agent on the copper exchanged α-Zr(PO4)2, dispersed on the polymeric matrix, allows the formation of copper metallic nanoparticles with 5-10 nm size • The metal nanoparticles are dispersed, as well as the fillers, over the entire polymer • A film of metallic copper with nanometrical dimensions is also present on the polymer surface • The size of nanoparticles on the surface of the samples is larger than the size of those placed inside the polymer In the future • Composites containing PVDF with Co, Ni and Fe with possible magnetic properties have been prepared • Preparation of nanocomposites containing other metal atoms (Ag and Pt) • Preparation of composites with polymers with enhanced thermal stability (Teflon or polystyrene) INSTM – Perugia 12-15 Giugno 2007

  16. Thanks for your kind attention Staff: Prof. G. Alberti Prof. U. Costantino Prof. M. Casciola Prof. R. Vivani Dr. F. Marmottini Dr.ssa M. Nocchetti Dr.ssa M. Pica (Ph D) Dr. F. Costantino (Ph D) Dr.ssa F. Montanari (Ph D) Dr. M. Sisani (Ph D student) Dr.ssa A. Donnadio (Ph D) Dr. M. Sganappa (Ph D student) Dr. R. Narducci (fellowship) Sig. R. Giulietti (technician) RESEARCH GROUP Laboratorio di Chimica Inorganica Dipartimento di Chimica Università di Perugia

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