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ELECTROSPUN NANOHYBRID MEMBRANES BASED ON BIORESORBABLE POLYMER AND CARBON NANOSTRUCTURES

ELECTROSPUN NANOHYBRID MEMBRANES BASED ON BIORESORBABLE POLYMER AND CARBON NANOSTRUCTURES. Ilaria Armentano , Alessandra Bianco, Costantino Del Gaudio, Mariaserena Dottori, Francesca Nanni, Josè Maria Kenny. Materials Engineering Centre, UdR INSTM, NIPLAB, University of Perugia, Terni,

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ELECTROSPUN NANOHYBRID MEMBRANES BASED ON BIORESORBABLE POLYMER AND CARBON NANOSTRUCTURES

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  1. ELECTROSPUN NANOHYBRID MEMBRANES BASED ON BIORESORBABLE POLYMER AND CARBON NANOSTRUCTURES Ilaria Armentano, Alessandra Bianco, Costantino Del Gaudio, Mariaserena Dottori, Francesca Nanni, Josè Maria Kenny. Materials Engineering Centre, UdR INSTM, NIPLAB, University of Perugia, Terni, Dip. di Scienze e Tecnologie Chimiche, Università di Roma Tor Vergata, Via della Ricerca Scientifica, Roma, 00133 (M) - ITALY VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  2. Aim The purpose of this study was to investigate nanohybrid systems based on bioresorbable Polymers and CNSs, in different Morphological structures. • Composition • Morphology VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  3. Outline • State of the art • Materials & Methods • Nanocomposite Development: Membranes & Film • Nanocomposite Charaterization: Morphological & Thermal & Dynamo-Mechanical • Conclusions VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  4. n n Bioresorbable Polymers PGA PLA PCL PLA-PGA PLA-PCL NANOCOMPOSITE • Chen G-X, Kim H-S, Park BH, Yoon J-S. Controlled Functionalization of Multiwalled Carbon Nanotubes with Various Molecular-Weight Poly(L-lactic acid)., J Phys Chem B 2005;109:22237-22243. • Zhongkui Honga, Xueyu Qiua, Jingru Suna, Mingxiao Denga, Xuesi Chena,b,*, Xiabin Jinga Grafting polymerization of L-lactide on the surface of hydroxyapatite nano-crystals, Polymer 45 (2004) 6699–6706 VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  5. Carbon Nanotubes tubes made of a single sheet of graphene (SingleWallNanoTube) or more sheets (MultiWallNanoTube) The regular geometry gives CNT excellent mechanical and electrical properties. CNT diameters are in the range 1 - 500 nm; CNT lengths can range from several µm to mm. Richard Smalley: “These nanotubes are so beautiful that they must be useful for something.” VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  6. Unique Structure CNTs Why CNTs? Extraordinary properties • Nano and um dimensions • High aspect ratio: 1000 • High specific surface area: 1400m2/g • High ratio interfacial area/vol: 1000 um-1 • Large number density/vol: 106 CNTs/um3 • Size scale comparable to interface layer (1-10 nm) • Chirality based on rolling direction • Found as single wall and Multi wall tubes Structure VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  7. Light, strong and highly flexible material Mechanical Properties Young’s modulus • SWNTs: 0.32-1.47 TPa (100 x steel) 0.5-5.5 TPa • SWNTs Bundles: 230 Gpa CNTs Fibres Vigolo B,Pe ｴnicaud A,Coulon C,Sauder C,Pailler R,Journet Cal.Macroscopic .bers and ribbons of oriented carbon nanotubes.Science 2000;290:1331. *C.A. Dyke and J.M. Tour. Covalent Functionalization ofSingle-Walled Carbon Nanotubes for Materials Applications.The Journal of Physical Chemistry, 2004. VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  8. ElectroSpinning A high voltage is applied to the solution such that at a critical voltage, typically more than 5 kV, the repulsive force within the charged solution is larger than its surface tension and a jet would erupt from the tip of the spinneret. Nanofibres The formation of nanofibres through electrospinning is based on the uniaxial stretching of a viscoelastic solution. DC > 5 kV Fibres Diameter A typical electrospinning set-up using a grounded static collector. • Experimental conditions: • Solution viscosity • Molecular weight • Voltage • Solvent Nanotechnology 17 (2006) R89–R106 WETeoand S Ramakrishna VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  9. Materials Polymer Matrix CNSs & CNFs: Carbon NanoFibers, Pyrograf ε-PCL Sigma Aldrich 1 % wt SWNTs:Single Wall Carbon Nanotubes, Thomas Swan & Co.Ltd. MW 80000 Methods Solvent Casting in CHCl3 Electrospinning Porous Membranes Flat Film d=200 µm • Chen G-X, Kim H-S, Park BH, Yoon J-S. Controlled Functionalization of Multiwalled Carbon Nanotubes with Various Molecular-Weight Poly(L-lactic acid)., J Phys Chem B 2005;109:22237-22243. • Zhongkui Honga, Xueyu Qiua, Jingru Suna, Mingxiao Denga, Xuesi Chena,b,*, Xiabin Jinga Grafting polymerization of L-lactide on the surface of hydroxyapatite nano-crystals, Polymer 45 (2004) 6699–6706 VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  10. SWNTs TGA In Air 5°C/min (30-1000)°C Seiko exstar 6000 FESEM - Zeiss Supra25 TG and derivative oxidation thermograms of pristineSWNTs SEM image of the specimen of pristine SWNTs cross linked bundles PURITY VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali T=555°C Residual Mass=3% Metal catalist

  11. CNFs Carbon Nanofibers FESEM - Zeiss Supra25 TGA In Air 5°C/min (30-1000)°C Seiko exstar 6000 VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  12. Morphological Analysis Field Emission Scanning Electron Microscopy FESEM-Supra 25 Zeiss PCL Membranes VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  13. CONTACT ANGLE Surface Characterization FTA 1000 Analyser Water PCL Membranes PCL Film (118± 1)° (74.5± 0.5)° hydrophobic surface VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  14. Morphological Analysis Field Emission Scanning Electron Microscopy FESEM-Supra 25 Zeiss Film, fracture surface PCL+ CNFs 1% wt VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  15. Morphological Analysis Field Emission Scanning Electron Microscopy FESEM-Supra 25 Zeiss Film, fracture surface PCL+ SWNTs 1% wt VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  16. Morphological Analysis Field Emission Scanning Electron Microscopy FESEM-Supra 25 Zeiss PCL+ CNFs 1% wt Surface Nanohybrid Membranes VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  17. Morphological Analysis Field Emission Scanning Electron Microscopy FESEM-Supra 25 Zeiss Nanohybrid Membranes PCL+ CNFs 1% wt Cross Section VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  18. Morphological Analysis Field Emission Scanning Electron Microscopy FESEM-Supra 25 Zeiss Nanohybrid Membranes PCL+ SWNTs 1% wt Surface VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  19. Cu Cu Dielectric Characterization Characterization of conductivity of CNSs/polymer materials: HP4284 20 Hz-1MHz An introduction of carbon nanotubes in the polymer matrix is expected to influence the strength and the electrical conductivity of the nanocomposite. PCL Nanocomposite Specific bulk AC conductivity and dielectric constant as a function of frequency forPCL based nanocomposite films with different nanofiller content. VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  20. Thermal Characterization DSC Mettler Toledo 822 DSC The samples were heated from -25 to 100°C at a scanning rate of 10°C/min. Two heating cycles were performed. The first heating cycle was used to remove all thermal history. PCL + CNSs Film VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  21. Thermal Characterization DSC Mettler Toledo 822 DSC The samples were heated from -25 to 100°C at a scanning rate of 10°C/min. Two heating cycles were performed. The first heating cycle was used to remove all thermal history. PCL + CNSs Membranes VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  22. Thermal Characterization Xc(%)=ΔH/ΔH0 ΔH0 = 136 J/g VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali Polymer 41 (2000) 9073–9080

  23. Thermal Characterization Seiko exstar 6000 TGA Film Membranes Td=404°C 30°C -> 1000°C, 10°C/min Nitrogen VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  24. Dynamo-Mechanical Characterization DMA: Dynamo-Mechanical AnalysisReometric Scientific-ARES N2 Dynamic Time Sweep Test f=1Hz Strain=0.3 DMA Film VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  25. CONCLUSIONS • Nanocomposites made with bioresorbable PCL matrix and CNSs were processed by solvent casting technique and electrospinning. • Objective: to analyze the effects of the incorporation of CNSs and their morphology on the Thermal, Mechanical and Electrical Properties • Hydrophobic surface induced by membrane process • CNSs serve the role of a plasticizer and a crystal nucleate, which enhances the polymer segmental mobility and facilitates the crystal packing simultaneously. • Elastic modulus increases significantly with introduction of CNSs in the polymer matrix. • An introduction of CNTs in the polymer matrix affects the electrical conductivity of the nanocomposite. • These studies suggest that the combination of biodegradable polymers and carbon nanostructures, opens in fact a new perspective in the self-assembly of nanomaterials and nanodevices with tunable mechanical and electrical properties. VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  26. Acknowlodgement VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

  27. Thank You!! VI Convegno Nazionale sulla Scienza e Tecnologia dei Materiali

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