Hydroxyapatite Mineralization on the Calcium Chloride Blended Polyurethane Nanofiber via Biomimetic Method

Polyurethane nanofibers containing calcium chloride (CaCl2) were prepared via an electrospinning technique for the biomedical applications. Polyurethane nanofibers with different concentration of CaCl2 were electrospun, and their bioactivity evaluation was conducted by incubating in biomimetic simulated body fluid (SBF) solution. The morphology, structure and thermal properties of the polyurethane/CaCl2 composite nanofibers were characterized by means of scanning electron microscopy (SEM), field-emission scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, Fourier transform infrared spectroscopy and thermogravimetry. SEM images revealed that the CaCl2 salt incorporated homogeneously to form well-oriented nanofibers with smooth surface and uniform diameters along their lengths. The SBF incubation test confirmed the formation of apatite-like materials, exhibiting enhanced bioactive behavior of the polyurethane/CaCl2 composite nanofibers. This study demonstrated that the electrospun polyurethane containing CaCl2 composite nanofibers enhanced the in vitro bioactivity and supports the growth of apatite-like materials.     

Fabrication and characterization of silver nanoparticle-incorporated bilayer electrospun–melt-blown micro/nanofibrous membrane

In this study, we fabricated an antifouling bilayered fibrous filter media having micro-nonwoven by melt blowing and nano-nonwoven by electrospinning process. Silver nanoparticle-incorporated polyurethane nanofibers were electrospun on the meltblown fiber of polypropylene. Silver nanoparticles were synthesized in situ in the polyurethane electrospun nanofibers through reduction of silver nitrate. The filter media were characterized by field emission scanning electron microscope, transmission electron microscopy, and X-ray diffraction and energy-dispersive X-ray spectroscopy analyses. The composite membrane showed that a thin layer of electrospun nanofibers improved the filtration efficiency without substantial increase in pressure drop. In situ synthesis of Ag NPs imparted the antibacterial and antifouling characteristics to the membrane.     

Antibacterial ciprofloxacin HCl incorporated polyurethane composite nanofibers via electrospinning for biomedical applications

We report on the preparation and characterization of polyurethane (PU) composite nanofibers by electrospinning. Two different approaches were adopted to obtain the PU composite nanofibers. In the first approach, a homogeneous solution of 10 wt% PU containing ciprofloxacin HCl (CipHCl) drug was electrospun to obtain PU/Drug composite nanofibers. And in the second approach, the PU with ciprofloxacin HCl drug and ceramic hydroxyapatite (HA) particles were electrospun to obtain the PU/Drug and PU/Drug/HA composite nanofibers. The surface morphology, structure, bonding configuration, optical and thermal properties of the resultant products were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and UV–vis spectroscopy. The antibacterial activity was tested against common food borne pathogenic bacteria, namely, Staphylococcus aureus, Escherichia coli by the minimum inhibitory concentration (MIC) method. Our result results demonstrate that these composite nanofibers possess superior characteristics which can utilized for variety of applications.     

Preparation and characterization of electrospun Ag/polyacrylonitrile composite nanofibers

Novel composite nanofibers consisting of Ag nanoparticles and polyacrylonitrile (PAN) were fabricated successfully. The Raman properties of these Ag/PAN nanofibers were studied at low temperatures, which showed good Raman characteristics. In the process, a PAN solution containing Ag ions was directly electrospun to obtain nanofiber films containing Ag ions, and the Ag ions of resulting composite nanofibers were reduced to Ag nanoparticles in N₂H₅OH aqueous solution. Then, we treated Ag/PAN composite nanofibers at 100 °C, 200 °C, 400 and 600 °C, respectively. The Ag/PAN nanocomposite film was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) patterns and surface-enhanced Raman scattering (SERS) spectroscopy.     

Antimicrobial activity of electrospun polyurethane nanofibers containing composite materials

We report on the preparation and characterization of electrospun polyurethane nanofibers containing silver, cactus, rosin and Scutellariae Radix. The utilized polyurethane nanofibers containing different composite materials were prepared by a simple dip coating method. The morphology, structure and thermal characteristics of as-prepared composite nanofibers were studied by scanning electron microscopy, X-ray diffraction, Fourier transform infrared, Raman spectroscopy and thermogravimetric analysis. The antimicrobial activity of the composite nanofibers was tested against two common food borne pathogenic bacteria, Staphylococcus aureus and Escherichia coli, by the minimum inhibitory concentration method. Our results demonstrated that more pronounced antimicrobial activities were observed for the composite nanofibers. Overall, the fabrication of cheap, stable and effective material with excellent antimicrobial activity can be utilized to inhibit the microbial growth associated with food stuff.     

Structural Behavior and In Vitro Bioactivity Evaluation of Sol-Gel Derived Glass-Ceramics Based on SiO<Subscript>2</Subscript>- CaO- P<Subscript>2</Subscript>O<Subscript>5</Subscript>- ZnO System

Glass and glass-ceramics, which are important bioceramics, have established an essential group of silicon-based materials having wide applications in medicine. Bioactive glass-ceramics have proved to be able to chemically bond to living bones due to forming an apatite-like layer on their surfaces. In this study, bioactive glass-ceramics of (64-X) SiO₂- 31 CaO- 5 P₂O₅- X ZnO based on mol% were synthesized by the sol–gel process. The bioactive glass-ceramics were analyzed using X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) before and after being exposed to simulated body fluid (SBF) solution. The results show that an increase in ZnO will cause the ability of calcium phosphate apatite formation on the glass-ceramic surfaces to first rise by 8 % but subsequently to decline by 12 %. The bioactivity of synthesized glass-ceramics can be confirmed by SEM and XRD due to the presence of a rich bone-like apatite layer.     

Bimetallic Zn/Ag doped polyurethane spider net composite nanofibers: A novel multipurpose electrospun mat

The objective of this study was to develop a new class of bimetallic ZnO/Ag embedded polyurethane multi-functional nanocomposite by a straightforward approach. Bimetallic nanomaterials, composed of two unlike metal elements, are of greater interest than the monometallic materials because of their improved characteristics. In the present study the bimetallic composite was prepared using sol–gel via the facile electrospinning technique. The utilized sol–gel was composed of zinc oxide, silver and poly(urethane). The physicochemical properties of as-spun composite mats were determined by X-ray diffraction pattern, field emission scanning electron microscopy, energy dispersive X-ray spectroscopy and transmission electron microscopy. The antibacterial activity was tested using Escherichia coli as model organism. The antibacterial test showed that ZnO:Ag/polyurethane composite possesses superior antimicrobial activity than pristine PU and ZnO/PU hybrids. Furthermore, our results illustrate that the synergistic effect of ZnO and Ag resulted in the advanced antimicrobial action of bimetallic ZnO/Ag composite mat. The viability and proliferation properties of NIH 3T3 mouse fibroblast cells on the ZnO:Ag/polyurethane composite nanofibers were analyzed by in vitro cell compatibility test. Our results indicated the non-cytotoxic behavior of bimetallic ZnO:Ag/polyurethane nanofibers towards the fibroblast cell culture. In summary, novel ZnO:Ag/polyurethane composite nanofibers which possess large surface to volume ratio with excellent antimicrobial activity were fabricated. The unique combination of ZnO and Ag nanoparticles displayed potent bactericidal effect due to a synergism. Hence the electrospun bimetallic composite indicates the huge potential in water filtration, clinical and biomedical applications.     

Preparation of porous nylon 6 fiber via electrospinning

Porous nylon‐6 fibers were obtained by electrospinning of ultra‐high molecular polyamide 6 (UHMW‐PA6). First, UHMW‐PA6/calcium formate composite nanofibers were prepared as precursors by electrospinning UHMW‐PA6 solutions containing different contents of calcium formate particles. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to examine the surface morphology and inner structure of composite nanofibers. It was found that calcium formate particles were distributed both inside and on the surface of nanofibers. Fourier transform infrared (FTIR), differential scanning calorimetry, and thermal gravimetric analysis (TGA) were used to study the structure and properties of these nanofibers. Then, porous UHMW‐PA6 nanofibers were obtained by soaking the electrospun web in water for 24 h, to remove calcium formate particles. The removal of calcium formate particles was confirmed using FTIR and TGA tests. SEM and TEM observations revealed the formation of porous structure in these nanofibers. In addition, CaCl₂ was used instead of calcium formate to prepare the UHMW‐PA6 nanoporous fiber. POLYM. ENG. SCI., 55:1133–1141, 2015. © 2014 Society of Plastics Engineers     

In vitro biocompatibility of a nanocrystalline β-Ta2O5 coating for orthopaedic implants

To improve the durability and bioactivity of Ti–6Al–4V alloy used for medical implants, the β-Ta₂O₅ nano-crystalline coatings were introduced using double cathode glow discharge technique. The coating microstructure was characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM). The coating exhibits an assembly of near-equiaxed grains, locally aligned normal to the coating surface. The β-Ta₂O₅ coating exhibits strong adhesion to substrate and a strong resistance to deformation and cracking under applied loads. Cells culture tests showed that the coating is more beneficial to the adhesion and proliferation of NIH-3T3 cells as compared to the uncoated alloy. In-vitro bioactivity was evaluated by immersion of the coating in simulated body fluids (SBF) for different periods up to 14 days at 37 °C. The results indicated that bioactivity of Ti–6Al–4V was dramatically improved after the deposition of β-Ta₂O₅, since the coating has a higher apatite forming ability than the Ti–6Al–4V substrate. Finally, the electrochemical behavior of the β-Ta₂O₅ coating after soaking in SBF at 37 °C for 0, 3, 7, and 14 days was studied through potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). EIS measurements also confirm that the presence of a hydroxyapatite layer on the coating becomes thicker and denser during soaking in SBF. Moreover, the coating exhibits better corrosion resistance than the bare alloy. Hence, the β-Ta₂O₅ coating is a promising candidate coating for protection of orthopedic implants with enhanced bioactivity and corrosion resistance.     

Fabrication of SiO2-ZrO2 composite fiber mats via electrospinning

(1 ? x)SiO₂-(x)ZrO₂ (x = 0.1, 0.2) composite fiber mats were prepared by electrospinning their sol-gel precursors of zirconium acetate and tetraethyl orthosilicate (TEOS) without using a polymer binder. The electrospun composite fibers were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), fourier transform infrared spectroscopy (FT-IR) and mercury porosimetry. The composite fibers having a tetragonal crystalline ZrO₂ were obtained by calcining the electrospun composite fibers at high temperatures. The results show that the structure and crystallization of ZrO₂ in the composite fibers can be controlled by sintering temperature, while the porosity and morphology of the fiber mats did not depend on the sintering temperature.     

Preparation and properties of PET/SiO2 composite micro/nanofibers by a laser melt-electrospinning system

Poly(ethylene terephthalate) (PET)/SiO₂ composite micro/nanofibers were successfully prepared by a laser melt-electrospinning system. The fibers with diameter ranging from 500 nm to 7 μm were obtained. The effect of laser current and applied voltage on the fibers morphologies was investigated by scanning electron microscopy (SEM), and the results showed that the relationship of process parameters and fibers diameter was complicated. The EDS analysis confirmed the presence of SiO₂ in the PET fibers matrix. The crystallization behavior of the electrospun PET/SiO₂ micro/nanofibers was investigated using X-ray diffraction (XRD) analysis and differential scanning calorimetry (DSC), and it was found that the as-electrospun fibers exhibited an amorphous phase. After heat-treatment at 120 and 160°C for 1 h, respectively, the fibers showed a high crystallinity. The thermal properties of fibers were studied using thermogravimetry-differential thermal analysis (TG–DTA), and showed the electrospun PET/SiO₂ composite fibers was not effective difference of thermostability compared with PET fibers when used for fibers materials. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Fabrication of antibacterial silver nanoparticle‐modified chitosan fibers using Eucalyptus extract as a reducing agent

Green chemical method could be a promising route to achieve large scale synthesis of nanostructures for biomedical applications. Here, we describe a green chemical synthesis of silver nanoparticles (Ag NPs) on chitosan‐based electrospun nanofibers using Eucalyptus leaf extract. A series of silver salt (AgNO₃) amounts were added to a certain composition of chitosan/polyethylene oxide aqueous acetic acid solution. The solutions were then electrospun to obtain nanofibrous mats and then, morphology and size of nanofibers were analyzed by scanning electron microscopy (SEM). Incubation of AgNO₃‐containing mats into Eucalyptus leaf extract led to the formation of Ag NP clusters with average diameter of 91 ± 24 nm, depicted by SEM and transmission electron microscopy. Surface enhanced Raman spectroscopy also confirmed formation of Ag NPs on the nanofibers. The mats also showed antimicrobial activity against Escherichia coli and Staphylococcus aureus bacteria with bigger inhibition zone for extract‐exposed mats against S. aureus. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42133.     

Studies on the synthesis of electrospun PAN‐Ag composite nanofibers for antibacterial application

We have successfully synthesized polyacrylonitrile (PAN) nanofibers impregnated with Ag nanoparticles by electrospinning method at room temperature. Briefly, the PAN‐Ag composite nanofibers were prepared by electrospinning PAN (10% w/v) in dimethyl formamide (DMF) solvent containing silver nitrate (AgNO₃) in the amounts of 8% by weight of PAN. The silver ions were reduced into silver particles in three different methods i.e., by refluxing the solution before electrospinning, treating with sodium borohydride (NaBH₄), as reducing agent, and heating the prepared composite nanofibers at 160°C. The prepared PAN nanofibers functionalized with Ag nanoparticles were characterized by field emission scanning electron microscopy (FESEM), SEM elemental detection X‐ray analysis (SEM‐EDAX), transmission electron microscopy (TEM), and ultraviolet‐visible spectroscopy (UV‐VIS) analytical techniques. UV‐VIS spectra analysis showed distinct absorption band at 410 nm, suggesting the formation of Ag nanoparticles. TEM micrographs confirmed homogeneous dispersion of Ag nanoparticles on the surface of PAN nanofibers, and particle diameter was found to be 5–15 nm. It was found that all the three electrospun PAN‐Ag composite nanofibers showed strong antibacterial activity toward both gram positive and gram negative bacteria. However, the antibacterial activity of PAN‐Ag composite nanofibers membrane prepared by refluxed method was most prominent against S. aureus bacteria. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Morphology enhancement of TiO2/PVP composite nanofibers based on solution viscosity and processing parameters of electrospinning method

In this work, different sol solutions with various titanium tetraisopropoxide (TIP)/glacial acetic acid ratios in 2‐propanol with 5 wt % poly(vinyl pyrrolidone) (PVP) (M_w = 360,000 g/mol) were prepared and electrospun. Composition of the prepared sols and as‐spun TiO₂/PVP nanofibers were determined by Fourier transform infrared and Raman spectroscopy methods. Morphology of the electrospun TiO₂/PVP nanofibers was studied by scanning electron microscopy and transmission electron microscopy (TEM) techniques. Rheometry measurements of the sol solutions showed decrease of viscosity upon the addition of TIP to the polymer solutions with constant polymer and acid concentrations. The sol solution having the lowest viscosity (at shear rate 10 s^?1) but the highest TIP/glacial acetic acid ratio showed beaded nanofibers morphology when electrospun under 10 and 12 kV applied voltage while injection rate, needle tip to collector distance, and needle gauge were kept constant. However, smooth electrospun TiO₂/PVP composite nanofibers with the average nanofibers diameters (148 ± 79 nm) were achieved under the same condition when applied voltage increased to 15 kV. TEM micrographs of the electrospun TiO₂/PVP nanofiber showed that the TiO₂ particles with continuous structure are formed at the middle of the nanofiber and distributed along its axis. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46337.     

In vitro apatite-forming ability of calcium aluminate blends

Calcium aluminate cement (CAC) blends show great potential as biomaterial when compared to commercial products used in odontology and orthopedics. Mixtures of CAC +4 wt% of different additives (alumina, zirconia, zinc oxide, tricalcium phosphate or hydroxyapatite) containing compositions, resulted in samples with low porosity levels and smaller pore sizes after their contact with simulated body fluid (SBF) solution, which was associated with apatite precipitation on the materials’ surface. In order to certify these aspects, the in vitro apatite-formation ability (bioactivity) of CAC blends was evaluated by pH and calcium concentration measurements in SBF for samples previously treated (or not) with sodium silicate (SS) solution. The surface of the samples after immersion in SBF or SBF/SS was analyzed by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analysis and confocal Raman spectroscopy. In addition, the in vitro apatite deposition and the osteoblastic cell viability were also evaluated. SEM results showed that the precipitation of phases was detected on the CAC blend samples’ surfaces. The presence of calcium and mainly phosphorus by EDX indicated the formation of calcium phosphate phases. Moreover, the presence of a more homogeneous apatite-like layer on the samples’ surface was observed after treatment with sodium silicate solution. The detection of the Raman signature at 960 cm⁻¹, confirmed the presence of an apatite-like layer on the surface of the compositions after immersion in SBF or SBF/SS. Regarding the osteoblastic cell viability results, blends with collagen, zinc oxide and zirconia presented better results when compared to commercial products.     

Fabrication of SiO2-ZrO2 composite fiber mats via electrospinning

(1 − x)SiO₂-(x)ZrO₂ (x = 0.1, 0.2) composite fiber mats were prepared by electrospinning their sol-gel precursors of zirconium acetate and tetraethyl orthosilicate (TEOS) without using a polymer binder. The electrospun composite fibers were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), fourier transform infrared spectroscopy (FT-IR) and mercury porosimetry. The composite fibers having a tetragonal crystalline ZrO₂ were obtained by calcining the electrospun composite fibers at high temperatures. The results show that the structure and crystallization of ZrO₂ in the composite fibers can be controlled by sintering temperature, while the porosity and morphology of the fiber mats did not depend on the sintering temperature.     

Electromagnetic properties of electrospun Fe3O4/carbon composite nanofibers

In order to develop multifunctional nanofibers, the electrical conductivity and magnetic properties of Fe₃O₄/carbon composite nanofibers have been examined. Polyacrylonitrile (PAN) is used as a matrix to produce magnetic composite nanofibers containing different amounts of magnetite (Fe₃O₄) nanoparticles. Electrospun composite nanofibers were thermally treated to produce electrically conductive and magnetically permeable composite carbon nanofibers. The composite nanofibers were characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD), Raman spectroscopy, four-point probe and Superconducting Quantum Interference Device (SQUID). Uniform nanofibers were obtained with successful transferring of magnetic properties of Fe₃O₄ into the as-spun composite nanofibers. The electromagnetic properties were tuned by adjusting the amount of Fe₃O₄ in the matrix and carbonization process. The electrical conductivity, magnetic moment and also magnetic hysteresis rise up by adding Fe₃O₄ and increasing carbonization temperature. The high surface area provided by the ultrafine fibrous structures, the flexibility and tuneable electromagnetic properties are expected to enable the expansion of the design options for a wide rage of electronic devices.     

The optical properties of PVA/TiO2 composite nanofibers

The electrospun nanofibers emerge several advantages because of extremely high specific surface area and small pore size. This work studies the effect of PVA nanofibers diameter and nano‐sized TiO₂ on optical properties as reflectivity of light and color of a nanostructure assembly consisting polyvinyl alcohol and titanium dioxide (PVA/TiO₂) composite nanofibers prepared by electrospinning technique. The PVA/TiO₂ composite spinning solution was prepared through incorporation of TiO₂ nanoparticles as inorganic optical filler in polyvinyl alcohol (PVA) solution as an organic substrate using the ultrasonication method. The morphological and optical properties of collected composites nanofibers were highlighted using scanning electron microscopy (SEM) and reflective spectrophotometer (RS). The reflectance spectra indicated the less reflectance and lightness of composite with higher nanofiber diameter. Also, the reflectance and lightness of nanofibers decreased with increasing nano‐TiO₂ concentration. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Bone substitute of poly(amino acid)/β‐Ca2SiO4 biocomposite: Degradability and bioactivity

A poly(amino acid)/β‐Ca₂SiO₄(PAA/β‐Ca₂SiO₄) bioactive composite was prepared by in situ melting polymerization. The composition, structure, and morphology were characterized by infrared spectrometry, X‐ray diffraction, X‐ray photoelectron spectroscopy, scanning electron microscopy, and differential scanning calorimeter. The results indicated that the β‐Ca₂SiO₄ particles were uniformly distributed in the PAA matrix and some interaction was found at the interface between PAA and β‐Ca₂SiO₄. The crystallinity of PAA in the composite was found decreasing with the increase of β‐Ca₂SiO₄ content. The bioactivity of the composite was evaluated by soaking the composite in simulated body fluid (SBF) and results showed that the PAA/β‐Ca₂SiO₄ composite (PSC) could induce a dense and continuous layer of apatite after soaking for 1 week. In addition, the PSC was soaked SBF for 2 months, and the weight loss reached 8.77%, showing the composite could be degradable. Collectively, these results suggested that the incorporation of β‐Ca₂SiO₄ produced a biocomposite with enhanced bioactivity and might have potential applications as a bone tissue substitute. POLYM. COMPOS., 37:1335–1341, 2016. © 2014 Society of Plastics Engineers     

Electrospun gelatin/nylon‐6 composite nanofibers for biomedical applications

We describe the preparation and characterization of gelatin‐containing nylon‐6 electrospun fibers and their potential use as a bioactive scaffold for tissue engineering. The physicochemical properties of gelatin/nylon‐6 composite nanofibers were analyzed using field emission scanning electron microscopy (FE‐SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, TGA and contact angle and tensile measurements. FE‐SEM and TEM images revealed that the nanofibers were well oriented and showed a good incorporation of gelatin. FTIR spectroscopy and TGA also revealed that there was good interaction between the two polymers at the molecular level. The adhesion, viability and proliferation properties of osteoblast cells on the gelatin/nylon‐6 composite nanofibers were analyzed by an in vitro cell compatibility test. Our results suggest that the incorporation of gelatin can increase the cell compatibility of nylon‐6 and therefore the composite mat obtained has great potential in hard tissue engineering. © 2012 Society of Chemical Industry