T. A. Kowalewski A. L. Yarin S. Błoński NANOFIBRES

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T. A. Kowalewski A. L. Yarin S. Błoński NANOFIBRES Institute of Fundamental Technological Research Polish Academy of Sciences & Department of Mechanical Engineering Technion - Israel Institute of Technology T. A. Kowalewski A. L. Yarin S. Błoński NANOFIBRES by electro-spinning of polymer solution

Nanofibres background Nanofibres properties Increase of the surface to volume ratio -> solar and light sails and mirrors in space Reduction of characteristic dimension -> nano-biotechnology, tissue engineering, chemical catalysts, electronic devices Bio-active fibres: catalysis of tissue cells growth Mechanical properties improvement -> new materials and composite materials by alignment in arrays and ropes Nanofibres production: Air-blast atomisation Pulling from melts Electrospinning of polymer solutions NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Classical liquid jet  0.1mm  Orifice – 0.1mm Primary jet diameter ~ 0.2mm Micro-jet diameter ~ 0.005mm Gravitational, mechanical or electrostatic pulling limited to l/d ~ 1000 by capillary instability To reach nano-range: jet thinning ~10-3 draw ratio ~106 ! NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Electro-spinning v=0.1m/s E ~ 105V/m moving charges e bending force on charge e E ~ 105V/m viscoelastic and surface tension resistance Moving charges (ions) interacting with electrostatic field amplify bending instability, surface tension and viscoelasticity counteract these forces NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Electro-spinning bending instability of electro-spun jet E ~ 105V/m charges moving along spiralling path E ~ 105V/m Bending instability enormously increases path of the jet, allowing to solve problem: how to decrease jet diameter 1000 times or more without increasing distance to tenths of kilometres NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Simple model for elongating viscoelastic thread Electro-spinning Simple model for elongating viscoelastic thread Stress balance:  - viscosity, G – elastic modulus stress,  stress tensor, dl/dt – thread elongation Momentum balance: Vo – voltage, e – charge, a – thread radius, h- distance pipette-collector Kinematic condition for thread velocity v Non-dimensional length of the thread as a function of electrostatic potential NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Nanofibres – basic setup liquid jet ~ 105 Volt/m NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Nanofibres – howto? Viscoelastic fluid: Dilute solution (4 – 6)% of polyethylene oxide (molar weight 4.105 g/mol), in 40% ethanol –water solvent Electrostatic field high voltage power supply (5-30kV) plastic syringe metal grid to collect fibres Visualization high speed camera (4000 – 40000 fps) high resolution „PIV” camera (1280x1024pixels) CW Argon laser, double pulse Nd:Yag laser, projection lens NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Nanofibres – basic setup NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Nanofibres collection NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Nanofibres collection NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Electrospinning observed at 30fps Average velocity of the fibres: 2 m/s 5 cm NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Electrospinning observed at 4500fps 0.0 ms 8.9 ms 17.8 ms 26.7 ms 35.6 ms 44.4 ms 53.3 ms 62.2 ms 71.1 ms 80.0 ms NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Electrospinning observed at 4500fps Average velocity of the fibre: 2 m/s 5 cm NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Electrospinning Collected nanofibres ------------ 10 mm ---------------  -0.1 mm- NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Electron microscopy PEO nanofibres NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Failure modes 0.5 mm NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Parametric study Model validation varying following parameters: L – length of the rectilinear part  – angle of the envelope cone (image analysis) U – velocity of the fibre by PIV method a – fibre diameter (image analysis) structure of collected woven (failure modes) elongation strength of single fibre measured by air jet Effect of Electrostatic potential V Distance pipette-collector H Solution concentration c Distance from the pipette x L  H NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Parametric study PIV cross – correlation t = 500 s image 2 t + t image 1 concentration of PEO: 3% Voltage: 8 kV H = 215 mm polymer solution with the addition of fluorescent particles (0.3m polymer microspheres) light source: Nd:Yag laser Average velocity of the fibres: 2 m/s NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Tested polymers Test Polymer Solvent Concentration Voltage [kV] Electrospinning I PEO Polyethylene-oxide 40% water – ethanol solution 3 – 4 % 3 – 12 good and stable process for voltage up to 10kV II DBC* Ethanol 2-29% 6 – 16 fairly good III TAC* 7-30 % 3 – 30 polymer too viscous 1-7 % 10 – 30 difficult IV PAN* DMF 1-25 % 5 – 25 very good *Prepared at Technical University of Łódź by dr Anna Błasińska NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Parametric study Polymer: PEO  Concentration: c=3% H Polymer: PEO Concentration: c=3% Solvent: 40% water- ethanol solution H=215mm V=8kV L (t) – instability of length of the rectilinear part NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Parametric study Polymer: PEO  Concentration: c=4% H Polymer: PEO Concentration: c=4% Solvent: 40% water- ethanol solution H=215mm L (V) – length of the rectilinear part  (V) – angle of the envelope cone NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Parametric study Polymer: PEO  Concentration: c=4% H Polymer: PEO Concentration: c=4% Solvent: 40% water- ethanol solution H=215mm U(V) – velocity of the fibre at the rectilinear part NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Electrospinning observed at 25fps Polymer: DBC Concentration: c=9% Solvent: ethanol H=215mm V=6kV 12 cm NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Different structure of spinning fibres for DBC polymer U=6kV U=12kV DBC: c=9% H=215mm NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Parametric study Polymer: DBC  Concentration: c=9% Solvent: ethanol H=215mm L (V) – length of the rectilinear part  (V) – angle of the envelope cone NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Electrospinning observed at 25fps Polymer: PAN Concentration: c=15% Solvent: DMF H=215mm V=13kV 12 cm NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Different structure of spinning fibres for PAN polymer U=13kV U=19kV PAN: c=15% H=215mm NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Parametric study Polymer: PAN  Concentration: c=15% Solvent: DMF H Polymer: PAN Concentration: c=15% Solvent: DMF H=215mm L (V) – length of the rectilinear part  (V) – angle of the envelope cone NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Comparison of PEO & DBC &PAN polymers L (V) – length of the rectilinear part  (V) – angle of the envelope cone NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Conclusions Electrostatic elongation of polymer threads allows to produce relatively easily fibres in nano range diameters Collection of nano-woven of bio-active polymers, e.g.. chitin may have practical application for tissue growth Electrospinning of polymer solutions still lacks detailed mathematical model, necessary to perform process optimisation NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse

Acknowledgements We would like to acknowledge the valuable contribution of dr Anna Błasińska from TU of Łódź and Anna Blim from IPPT PAN in the work presented. The work was partly supported by the Centre of Excellence AMAS of the IPPT PAN NANOFIBRES T. A. Kowalewski, A. L. Yarin & S. Błoński, EFMC 2003, Toulouse