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Wettability of electrospun fibers is one of the key parameters in the biomedical and filtration industry. Within this comprehensive study of contact angles on three-dimensional (3D) meshes made of electrospun fibers and films, from seven types of polymers, we clearly indicated the importance of roughness analysis. Surface chemistry was analyzed with X-ray photoelectron microscopy (XPS) and it showed no significant difference between fibers and films, confirming that the hydrophobic properties of the surfaces can be enhanced by just roughness without any chemical treatment. The surface geometry was determining factor in wetting contact angle analysis on electrospun meshes. We noted that it was very important how the geometry of electrospun surfaces was validated. The commonly used fiber diameter was not necessarily a convincing parameter unless it was correlated with the surface roughness or fraction of fibers or pores. Importantly, this study provides the guidelines to verify the surface free energy decrease with the fiber fraction for the meshes, to validate the changes in wetting contact angles. Eventually, the analysis suggested that meshes could maintain the entrapped air between fibers, decreasing surface free energies for polymers, which increased the contact angle for liquids with surface tension above the critical Wenzel level to maintain the Cassie-Baxter regime for hydrophobic surfaces.

Piezoelectric polymers are promising energy materials for wearable and implantable applications for replacing bulky batteries in small and flexible electronics. Therefore, many research studies are focused on understanding the behavior of polymers at a molecular level and designing new polymer-based generators using polyvinylidene fluoride (PVDF). In this work, we investigated the influence of voltage polarity and ambient relative humidity in electrospinning of PVDF for energy-harvesting applications. A multitechnique approach combining microscopy and spectroscopy was used to study the content of the β-phase and piezoelectric properties of PVDF fibers. We shed new light on β-phase crystallization in electrospun PVDF and showed the enhanced piezoelectric response of the PVDF fiber-based generator produced with the negative voltage polarity at a relative humidity of 60%. Above all, we proved that not only crystallinity but also surface chemistry is crucial for improving piezoelectric performance in PVDF fibers. Controlling relative humidity and voltage polarity increased the d 33 piezoelectric coefficient for PVDF fibers by more than three times and allowed us to generate a power density of 0.6 μW·cm –2 from PVDF membranes. This study showed that the electrospinning technique can be used as a single-step process for obtaining a vast spectrum of PVDF fibers exhibiting different physicochemical properties with β-phase crystallinity reaching up to 74%. The humidity and voltage polarity are critical factors in respect of chemistry of the material on piezoelectricity of PVDF fibers, which establishes a novel route to engineer materials for energy-harvesting and sensing applications.

This study represents the unique analysis of the electrospun scaffolds with the controlled and stable surface potential without any additional biochemical modifications for bone tissue regeneration. We controlled surface potential of polyvinylidene fluoride (PVDF) fibers with applied positive and negative voltage polarities during electrospinning, to obtain two types of scaffolds PVDF­(+) and, PVDF(−). The cells’ attachments to PVDF scaffolds were imaged in great details with advanced scanning electron microscopy (SEM) and 3D tomography based on focus ion beam (FIB-SEM). We presented the distinct variations in cells shapes and in filopodia and lamellipodia formation according to the surface potential of PVDF fibers that was verified with Kelvin probe force microscopy (KPFM). Notable, cells usually reach their maximum spread area through increased proliferation, suggesting the stronger adhesion, which was indeed double for PVDF(−) scaffolds having surface potential of −95 mV. Moreover, by tuning the surface potential of PVDF fibers, we were able to enhance collagen mineralization for possible use in bone regeneration. The scaffolds built of PVDF(−) fibers demonstrated the greater potential for bone regeneration than PVDF­(+), showing after 7 days in osteoblasts culture produce well-mineralized osteoid required for bone nodules. The collagen mineralization was confirmed with energy dispersive X-ray spectroscopy (EDX) and Sirius Red staining, additionally the cells proliferation with fluorescence microscopy and Alamar Blue assays. The scaffolds made of PVDF fibers with the similar surface potential to the cell membranes promoting bone growth for next-generation tissue scaffolds, which are on a high demand in bone regenerative medicine.

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