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Electrospinning and Nanofabrication for Health and Energy

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Electrospinning is a process allowing the elaboration of nanofibrous non-woven membranes (fiber diameter ≈ 50 nm up to 1 μm) from polymer solutions or molten polymers. We develop novel processes in order to control the structures at the scale of the nanofiber as well as at the scale of the membrane. Thanks to collaborations, the elaborated materials can be used for biomedical applications, sensors, catalysis or filters:

2D and 3D assemblies / Nanofibers for health

(Resp. Guy Schlatter)

We seek to control the organization of the nanofibers in the final material. This microstructuration allows the control of the porosity, the anisotropy of the fiber deposit (aligned fibers, stars,...) or even the chemical composition at the scale of few tens of microns. It will allow to open new applications (tissue engineering, composites, sensors,...). Some of these strategies were or are developped under the frame of ANR projects (ANR-P2N-2011-NeoTissage and ANR-DS03-2015-MimHeart).

The main collaborations  are established with INSERM allowing us to envisage several applications for tissue engineering or wound healing. We also develop different strategies to functionalize the surface of the nanofibers such as the grafting of peptides on polyrotaxane-based fibers (Project ANR-blanc 2011 FibRotaxanes) or thanks to the elaboration of coaxial fibers by the incorporation of drugs in the shell formulation (project in collaboration with UFSCAR, Sao Carlos, Brazil).

Open Access article: Link

Our team proposed a new process: the ETAD process (Electrostatic Template Assisted Deposition) allowing the elaboration of nanofibres/microparticules 2D microstructured composite membranes. The ETAD process was applied for the fabrication of biochips allowing the study of the effect of the membrane microstructure on the proliferation and mineralization of bone cells.

Ref: S. Nedjari, A. Hébraud, S. Eap, S. Siegwald, C. Mélart, N. Benkirane-Jessel, G. Schlatter, "Electrostatic Template-Assisted Deposition of Microparticles on Electrospun Nanofibers: Towards Microstructured Functional Biochips for Screening Applications", RSC Advances, vol. 5, pp. 83600-83607, 2015Link

2D structures obtained thanks to the use of micro-patterned collectors.

Ref: N. Lavielle et al. "Structuring and molding of electrospun nanofibers: Effect of electrical and topographical local properties of micro-patterned collectors ", Macromolecular Materials and Engineering, vol. 297, pp. 958-968, 2012. Link

Micro-structured honeycomb nanofibrous scaffolds. Effect of the structuration on the proliferation of bone cells (collaboration with INSERM-U1109).

Ref: S. Nedjari, S. Eap, A. Hébraud, C.R. Wittmer, N. Benkirane-Jessel, G. Schlatter, "Electrospun Honeycomb as Nests for Osteoblast Proliferation", Macromolecular Biosciencevol. 14, pp. 1580-1589, 2014Link

From self-assembled nanofibers to 3D porous cm-thick constructs: application for bone regeneration.

Ref: D. Ahirwal et al. "From Self-assembly of Electrospun NanoFibers to 3D cm-thick Hierarchical Foams", Soft Matter, vol. 9(11), pp. 3164-3172, 2013Link


3D structured composites made of nanofibres and microparticules obtained by ETAD process allowing controlled electrostatic interactions during alternate electrospinning and electrospraying on micro patterned collectors.

Ref: C.R. Wittmer, A. Hébraud, S. Nedjari, G. Schlatter, "Well-Organized 3D Nanofibrous Composite Constructs using Cooperative Effects between Electrospinning and Electrospraying", Polymer, vol. 55, pp. 5781-5787, 2014Link


Application of the process for the elaboration of biomimetic scaffolds for bone tissue engineering.

Ref: A. Garcia Garcia et al, "Poly(e-caprolactone) / hydroxyapatite 3D honeycomb scaffolds for a cellular microenvironment adapted to maxillofacial-bone reconstruction", ACS Biomaterials Science and Engineering, vol. 4, pp. 3317–3326, 2018Link


3D structures with controlled porosity gradient obtained by electrospinning on micropatterned collectors. a) Cross-section (x,z plane) of the membrane showing the porosity gradient. b) (x,y) planes obtained from X-ray micro-tomography for different z values. c,d) Mechanisms of the 3D structuration.

Ref: S. Nedjari, G. Schlatter, A. Hébraud, "Thick Honeycomb Electrospun Scaffold with Controlled Pore Size and Porosity Gradient", Materials Letters, vol. 142, pp. 180-183, 2015Link

Coaxial structure (PCL/gelatin/hydroxyapatite) of nanofibers for bone regeneration (collaboration with UFSCAR, Sao Carlos, Brazil).

Ref: I.H.L. Pereira, E. Ayres, L. Averous, G. Schlatter, A. Hébraud, A.C. Chagas de Paula, P. Henrique L. Viana, A.M. Goes, R.L. Oréfice, "Differentiation of human adipose-derived stem cells seeded on mineralized electrospun co-axial poly(caprolactone) (PCL) / gelatin nanofibers", Journal of Materials Science: Materials in Medicinevol. 25, pp. 1137-1148, 2014Link

 

 

 

Supramolecular materials: from the structures and the self-assembling properties to the processing

(Resp. Guy Schlatter)

Cyclodextrin-based materials

Polyrotaxanes (PR) are supramolecular necklaces used for the elaboration of functional materials or supramolecular gels with high mechanical properties and high swelling ratio. We focus on the synthesis of PR based on cyclodextrines (ring molecules of the necklace with 6, 7 or 8 glucose units) and polymers (forming the chain of the necklace) such as polyethylene oxyde (PEO), polypropylene oxyde (PPO), PEO-PPO-PEO block copolymers or poly(ε-caprolactone). We also focus on the self-assembling properties of PR and pseudo-PR and on their application for biomedical (project ANR-Blanc FibRotaxanes 2011-2014).
Furthermore, cyclodextrins are also used in the formulations for electrospinning in order to functionalize the nanofibers for drug encapsulation and controlled release purposes. Cyclodextrin is also a processing aid for electrospinning in aqueous solution.

Tannic acid based materials:

More recently, we started research activities dealing with the elaboration of materials from tannic acid, a molecule allowing the formation of supramolecular assemblies with metals by chelation.

We demonstrated that electrospinning of tannic acid in water without any polymer is possible thanks to the formation of a supramolecular network in the processed solution. Subsequently, the nanowebs can be efficiently cross-linked in water either by oxidative reaction with sodium periodate or, most interestingly, with Fe(III) by a combination of oxidative reaction and the formation of coordination complexes. The proposed strategy is easy, low cost, scalable and uses non-toxic solvents as well as biocompatible and biofunctional molecules paving thus the way for various applications in material and biomaterial sciences as well as in catalysis.

Ref: M. Allais, D. Mailley et al. "Polymer-free electrospinning of tannic acid and cross-linking in water for hybrid supramolecular nanofibres", Nanoscale, vol. 10, pp. 9164-9173, 2018Link.

 

Synthesis of pseudo-polyrotaxanes and their self-organization into nanoplatelets. Processing of the nanoplatelets by coaxial electrospinning and post-functiunalization of the nanofibers.

Ref: M. Oster, A. Hébraud, S. Gallet, A. Lapp, E. Pollet, L. Avérous, G. Schlatter, "Star-pseudopolyrotaxane organized in nanoplatelets for poly(ε-caprolactone)-based nanofibrous scaffolds with enhanced surface reactivity", Macromolecular Rapid Communications, vol. 36, pp. 292−297, 2015Link


M. Oster, G. Schlatter, S. Gallet, R. Baati, E. Pollet, C. Gaillard, L. Avérous, C. Fajolles, A. Hébraud, "Study of the pseudo-polyrotaxane architecture as a route for mild surface functionalization by click-chemistry of poly(ε-caprolactone)-based electrospun fibers", Journal of Materials Chemistry B, vol. 5, pp. 2181-2189, 2017Link

Nano-platelets of pseudo-polyrotaxanes based on β-CD and pluronics.

Ref: C. Perry et al. "Pluronic and β-cyclodextrin in water: from swollen micelles to self-assembled crystalline platelets", Soft Matter, vol. 7, pp. 3502-3512, 2011Link

 

Self-assembling of a polyrotaxane activated by the temperature.

Ref: C. Travelet et al. "Temperature-dependent structure of α-CD/PEO-based polyrotaxanes in concentrated solution in DMSO: kinetics and multiblock copolymer behaviour.", Macromolecules, vol. 43, pp. 1915–1921, 2010. Link

 

 

Functional nanofibers for energy, catalysis and sensors

(Resp. Anne Hébraud)

The goal of this research axis is the preparation and the characterization of functional organic, inorganic or hybrid nanofibers for energy, catalysis or sensors. Our approach starts from the chemistry (synthesis of semi-conductive conjugated polymers, sol-gel processes,...) to the elaboration and the characterization of devices (organic field effect transistors (OFET), sensors...) thanks to the available equipments (STnano clean room, organic electronics platform at team MaCÉPV from Icube and well-established collaborations with other teams of ICPEES. Thus, we are working on the fabrication of sensors made of composite nanofibers, the elaboration of TiO2-based photocatalytic nanofibrous materials (collaboration with the Department "Catalyse, Energie et Procédés" team: Photocatalyse et Photoconversion), carbon-based nanofibers (Department "Physico-Chimie des Nanosystèmes" team: Nanomatériaux, Catalyse et Interfaces) or the fabrication of membranes for fuel cells (PMNA-Région Alsace project supervised by the Electrochimie et Conversion d'Energie team of the "Catalyse, Energie et Procédés" Department).

Hierarchical carbon fiber / carbon nanofibers CF/CNF composite obtained by electrospinning / CVD for applications in catalysis: a) Example of a CF/CNF composite. b) Picture showing one single hairy carbon CF/CNF fiber. c) TEM showing CNFs at the surface of a CF embedding Ni0 nanoparticles.

(Collaboration with the Nanomatériaux, Catalyse et Interfaces team)

Ref: Y. Liu, J. Luo, C. Helleu, M. Behr, H. Ba, T. Romero, A. Hébraud, G. Schlatter, O. Ersen, D.S. Su, C. Pham-Huu, "Hierarchical porous carbon fibers/carbon nanofibers monolith from electrospinning/CVD processes as high effective surface area support platform", Journal of Materials Chemistry A, vol. 5, pp. 2151-2162, 2017 Link

Nitrogen-doped carbon porous nanofibers for oxidation of H2S to sulfur.

(Collaboration with the Nanomatériaux, Catalyse et Interfaces team)

Ref: Y. Liu et al.,"One-pot synthesis of nitrogen-doped carbon composite by electrospinning as metal-free catalyst for oxidation of H2S to sulfur", ChemCatChem, vol. 7, 2957-2964, 2015Link

TiO2 nanofibers obtained from sol-gel reactions (collaboration with the Photocatalyse et Photoconversion team)

Elaboration of semi-conductive fluorescent fibers by coaxial electrospinning.

Funders and industrial partners

Competitiveness clusters