Search results for: Crystallinity

Authors: Michael Sigruener, Dirk Muscat, Nicole Struebbe

Abstract:

Fiber reinforcement is a state of the art to enhance mechanical properties in plastics. For concrete and civil engineering, steel reinforcements are commonly used. Steel reinforcements show disadvantages in their chemical resistance and weight, whereas polymer fibers' major problems are in fiber-matrix adhesion and mechanical properties. In spite of these facts, longevity and easy handling, as well as chemical resistance motivate researches to develop a polymeric material for fiber reinforced concrete. Adhesion and interfacial mechanism in fiber-polymer-composites are already studied thoroughly. For polymer fibers used as concrete reinforcement, the bonding behavior still requires a deeper investigation. Therefore, several differing polymers (e.g., polypropylene (PP), polyamide 6 (PA6) and polyetheretherketone (PEEK)) were spun into fibers via single screw extrusion and monoaxial stretching. Fibers then were embedded in a concrete matrix, and Single-Fiber-Pull-Out-Tests (SFPT) were conducted to investigate bonding characteristics and microstructural interface of the composite. Differences in maximum pull-out-force, displacement and slope of the linear part of force vs displacement-function, which depicts the adhesion strength and the ductility of the interfacial bond were studied. In SFPT fiber, debonding is an inhomogeneous process, where the combination of interfacial bonding and friction mechanisms add up to a resulting value. Therefore, correlations between polymeric properties and pull-out-mechanisms have to be emphasized. To investigate these correlations, all fibers were introduced to a series of analysis such as differential scanning calorimetry (DSC), contact angle measurement, surface roughness and hardness analysis, tensile testing and scanning electron microscope (SEM). Of each polymer, smooth and abraded fibers were tested, first to simulate the abrasion and damage caused by a concrete mixing process and secondly to estimate the influence of mechanical anchoring of rough surfaces. In general, abraded fibers showed a significant increase in maximum pull-out-force due to better mechanical anchoring. Friction processes therefore play a major role to increase the maximum pull-out-force. The polymer hardness affects the tribological behavior and polymers with high hardness lead to lower surface roughness verified by SEM and surface roughness measurements. This concludes into a decreased maximum pull-out-force for hard polymers. High surface energy polymers show better interfacial bonding strength in general, which coincides with the conducted SFPT investigation. Polymers such as PEEK or PA6 show higher bonding strength in smooth and roughened fibers, revealed through high pull-out-force and concrete particles bonded on the fiber surface pictured via SEM analysis. The surface energy divides into dispersive and polar part, at which the slope is correlating with the polar part. Only polar polymers increase their SFPT-function slope due to better wetting abilities when showing a higher bonding area through rough surfaces. Hence, the maximum force and the bonding strength of an embedded fiber is a function of polarity, hardness, and consequently surface roughness. Other properties such as crystallinity or tensile strength do not affect bonding behavior. Through the conducted analysis, it is now feasible to understand and resolve different effects in pull-out-behavior step-by-step based on the polymer properties itself. This investigation developed a roadmap on how to engineer high adhering polymeric materials for fiber reinforcement of concrete.

Keywords: fiber-matrix interface, polymeric fibers, fiber reinforced concrete, single fiber pull-out test

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Authors: Piotr K. Szewczyk, Arkadiusz Gradys, Sungkyun Kim, Luana Persano, Mateusz M. Marzec, Oleksander Kryshtal, Andrzej Bernasik, Sohini Kar-Narayan, Pawel Sajkiewicz, Urszula Stachewicz

Abstract:

Piezoelectric polymers have received great attention in smart textiles, wearables, and flexible electronics. Their potential applications range from devices that could operate without traditional power sources, through self-powering sensors, up to implantable biosensors. Semi-crystalline PVDF is often proposed as the main candidate for industrial-scale applications as it exhibits exceptional energy harvesting efficiency compared to other polymers combined with high mechanical strength and thermal stability. Plenty of approaches have been proposed for obtaining PVDF rich in the desired β-phase with electric polling, thermal annealing, and mechanical stretching being the most prevalent. Electrospinning is a highly tunable technique that provides a one-step process of obtaining highly piezoelectric PVDF fibers without the need for post-treatment. In this study, voltage polarity and relative humidity influence on electrospun PVDF, fibers were investigated with the main focus on piezoelectric β-phase contents and piezoelectric performance. Morphology and internal structure of fibers were investigated using scanning (SEM) and transmission electron microscopy techniques (TEM). Fourier Transform Infrared Spectroscopy (FITR), wide-angle X-ray scattering (WAXS) and differential scanning calorimetry (DSC) were used to characterize the phase composition of electrospun PVDF. Additionally, surface chemistry was verified with X-ray photoelectron spectroscopy (XPS). Piezoelectric performance of individual electrospun PVDF fibers was measured using piezoresponse force microscopy (PFM), and the power output from meshes was analyzed via custom-built equipment. To prepare the solution for electrospinning, PVDF pellets were dissolved in dimethylacetamide and acetone solution in a 1:1 ratio to achieve a 24% solution. Fibers were electrospun with a constant voltage of +/-15kV applied to the stainless steel nozzle with the inner diameter of 0.8mm. The flow rate was kept constant at 6mlh⁻¹. The electrospinning of PVDF was performed at T = 25°C and relative humidity of 30 and 60% for PVDF30+/- and PVDF60+/- samples respectively in the environmental chamber. The SEM and TEM analysis of fibers produced at a lower relative humidity of 30% (PVDF30+/-) showed a smooth surface in opposition to fibers obtained at 60% relative humidity (PVDF60+/-), which had wrinkled surface and additionally internal voids. XPS results confirmed lower fluorine content at the surface of PVDF- fibers obtained by electrospinning with negative voltage polarity comparing to the PVDF+ obtained with positive voltage polarity. Changes in surface composition measured with XPS were found to influence the piezoelectric performance of obtained fibers what was further confirmed by PFM as well as by custom-built fiber-based piezoelectric generator. For PVDF60+/- samples humidity led to an increase of β-phase contents in PVDF fibers as confirmed by FTIR, WAXS, and DSC measurements, which showed almost two times higher concentrations of β-phase. A combination of negative voltage polarity with high relative humidity led to fibers with the highest β-phase contents and the best piezoelectric performance of all investigated samples. This study outlines the possibility to produce electrospun PVDF fibers with tunable piezoelectric performance in a one-step electrospinning process by controlling relative humidity and voltage polarity conditions. Acknowledgment: This research was conducted within the funding from m the Sonata Bis 5 project granted by National Science Centre, No 2015/18/E/ST5/00230, and supported by the infrastructure at International Centre of Electron Microscopy for Materials Science (IC-EM) at AGH University of Science and Technology. The PFM measurements were supported by an STSM Grant from COST Action CA17107.

Keywords: crystallinity, electrospinning, PVDF, voltage polarity

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