SHINSHU UNIVERSITY Shinshu University Nano Fusion Technology Research Group Study on the poly(1-butene) fibrous membrane via electrospinning Daisuke Kimura 키무라 다이수케

Shinshu University Nano Fusion Technology Research Group Introduction - Electrospinning - Poly(1-butene) - Goal of my study Experimental - preparation of samples - characterizations Results and discussions - SEM, WAXD, and DSC Conclusions Outline

Shinshu University Nano Fusion Technology Research Group Introduction Electrospinning Device for the solution electrospinning

Shinshu University Nano Fusion Technology Research Group Polyolefines Polyethylene Polypropylene Poly(1-butene) Poly(4-metyl-1-pentene) Polyolefines Insulation Mechanical strength Chemical stability Good point

Shinshu University Nano Fusion Technology Research Group Poly(1-butene) Structural formula of Poly(1-butene) Semi crystalline polymer PB has four different crystalline structure (I, I´, II, and III) PB crystalline structure has time-dipendent

Shinshu University Nano Fusion Technology Research Group Goal of my study It was difficult to prepare PB fibrous membrane via solution electrospinning process. Studies about crystalline properties of electrospun PB membrane were not so many. Preparing PB fibrous membrane and finding best condition of electrospinning Researching about crystalline transformation by mechanical deformation.

Shinshu University Nano Fusion Technology Research Group Experimental Applied voltage : 10kV Tip Collector Distance : 15cm Collector : Rotating drum Ambient temperature : RT Ambient humidity : about 40% Solution concentration : 0.5 %, 1.5 %, and 2.0 % (Each solution were stirred at 80 ℃ and then cooled to room temperature.) Preparation - electrospinning

Shinshu University Nano Fusion Technology Research Group Equipment : tensile tester Stretched length : 8 %, 16%, and 24 % Preparation - Stretching Initial length (100 %) Stretched 8% 16% 24%

Shinshu University Nano Fusion Technology Research Group SEM (Scanning electron microscopy) Which concentration is the best? Tensile test Elastic and plastic deformation range. WAXD (Wide angle X-ray diffraction) Evaluation about crystalline structure. DSC (Differential scanning calorimetry) Additional evaluation about crystalline structure. Characterizations

Shinshu University Nano Fusion Technology Research Group Results and discussions SEM images of PB membranes 0.50wt% 10.0μm 1.50wt% 10.0μm 2.50wt% 10.0μm SEM images of PB membranes

Shinshu University Nano Fusion Technology Research Group Tensile test Force (N) Deformation (mm) Force – Deformation curve of PB membranes (Initial sample size was 5cm) Elastic zone

Shinshu University Nano Fusion Technology Research Group 0%0% 20.0μm SEM images of stretched PB membranes 8%8% 20.0μm SEM images of stretched PB membranes 16 % 20.0μm 24 % 20.0μm 24% relaxed 20.0μm

Shinshu University Nano Fusion Technology Research Group Effect of stretching to fiber diameter Average diameters of each sample

Shinshu University Nano Fusion Technology Research Group Crystalline transformation - WAXD Structural formula of Poly(1-butene) theta E-Spun PB Membrane 8% Stretched 16% Stretched 24% Stretched 24% relaxed

Shinshu University Nano Fusion Technology Research Group Crystalline transformation - DSC Structural formula of Poly(1-butene) Temperature( ℃ ) Not stretched 24% relaxed Melting point of form I´ Melting point of form I

Shinshu University Nano Fusion Technology Research Group Conclusions We successfully prepared poly(1-butene) fibrous membrane via electrospinning. We observed and evaluated about stretched effect by SEM, WAXD, and DSC for the first time. It was observed that mechanical deformation caused crystalline transformation such as form II → form I by WAXD and DSC.