Preparation and antibacterial activity of polyvinyl alcohol/regenerated silk fibroin composite fibers containing Ag nanoparticles

Polyvinyl alcohol (PVA)/regenerated silk fibroin (SF)/AgNO₃ composite nanofibers were prepared by electrospinning. A large number of nanoparticles containing silver were generated in situ and well‐dispersed nanoparticles were confirmed by transmission electron microscopy (TEM) intuitionally. Ultraviolet (UV)‐visible spectroscopy and X‐ray diffraction (XRD) patterns indicated that nanoparticles containing Ag were present both in blend solution and in composite nanofibers after heat treatment and after subsequent UV irradiation. By annealing the nanofibers, Ag⁺ therein was reduced so as to produce nanoparticles containing silver. By combining heat treatment with UV irradiation, Ag⁺ was transformed into Ag clusters and further oxidized into Ag₃O₄ and Ag₂O₂. Especially size of the nanoparticles increased with heat treatment and subsequent UV irradiation. This indicated that the nanoparticles containing silver could be regulated by heat treatment and UV irradiation. The antimicrobial activity of heat‐treated composite nanofibers was evaluated by Halo test method and the resultant nanofibers showed very strong antimicrobial activity. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Photocatalytic Deposition of Silver Nanoparticles onto Organic/Inorganic Composite Nanofibers

Summary: In this work, silver nanoparticles were embedded in electrospun organic/inorganic composite nanofibers consisting of PAN and TiO₂ through photocatalytic reduction of the silver ions in silver nitrate solutions under UV irradiation. The morphology and diameter of PAN/TiO₂ composite nanofibers could be controlled by varying the initial contents of TiO₂ in the spinning solution. From TEM images and UV‐Vis spectra, it has been confirmed that monodisperse silver nanoparticles with a diameter of ≈2 nm were deposited selectively upon the titania of the as prepared composite nanofibers. The amount of Ag nanoparticles embedded on composite nanofibers was greatly influenced by the amount of TiO₂ in composite nanofibers, reflecting the role of titania as the inorganic stabilizer and photocatalyst.

Morphology of silver nanoparticles embedded on PAN/TiO₂ composite nanofibers.     

Electrospun antibacterial nylon nanofibers through in situ synthesis of nanosilver: preparation and characteristics

A new method for production of nylon nanofibers with antibacterial properties containing silver nanoparticles (nylon nanofibers/Ag NPs) is introduced via in situ synthesis of nano-silver by reduction of silver nitrate in the polymer solution prior to electrospinning. The properties of the electrospinning solutions and the structures of the electrospun fibers were studied using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDAX), UV?Cvis spectrophotometer and reflection spectrophotometer. Further, the antibacterial properties of the nanofibers were investigated against Escherichia coli (Gram-negative) and Staphylococcus aureus (Gram-positive) bacteria. Interestingly, an antibacterial properties has been found on nylon 6 nanofibers while the nylon nanofibers/Ag NPs showed excellent antibacterial activities against both tested bacteria. The produced nylon nanofibers/Ag NPs can be a good candidate for biomedical applications, water and air filtration.     

Preparation and characterization of poly(vinyl alcohol) cryogel‐silver nanocomposites and evaluation of blood compatibility,cytotoxicity, and antimicrobial behaviors

In this investigation, cryogels composed of poly(vinyl alcohol) (PVA) were prepared by repeated freeze‐thaw method. The prepared cryogels served as templates for producing highly stable and uniformly distributed silver nanoparticles via in situ reduction of silver nitrate (AgNO₃) using alkaline formaldehyde solution as reducing agent. The structure of the PVA/Ag cryogel nanocomposites was characterized by a Fourier transform infrared and Raman spectroscopy. The morphologies of pure PVA cryogels and PVA/Ag nanocomposites were observed by a scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques. The SEM analysis suggested that cryogels show a well defined porous morphology whereas TEM micrographs revealed the presence of nearly spherical and well separated Ag nanoparticles with diameter about 100 nm. XRD results showed all relevant Bragg's reflections for crystal structure of silver nanoparticles. The amount of silver in cryogel nanocomposites and thermal stability were determined by inductively coupled plasma atomic emission spectrometry (ICP‐AES) and thermogravimetric analysis measurements. Mechanical properties of nanocomposites were observed in terms of tensile strength. The antibacterial studies of the synthesized nanosilver containing cryogels showed good antibacterial activity against both gram‐negative and gram‐positive bacteria. The prepared PVA/Ag nanocomposites were also investigated for swelling and deswelling behaviors. The results reveal that both the swelling and deswelling process depends on the chemical composition of the cryogel silver nanocomposites, number of freeze‐Thaw cycles and pH and temperature of the swelling medium. The biocompatibility of the prepared nanocomposites was judged by in vitro methods of percent hemolysis and protein (BSA) adsorption. POLYM. COMPOS., 36:1983–1997, 2015. © 2014 Society of Plastics Engineer     

In situ preparation,electrospinning, and characterization of polyacrylonitrile nanofibers containing silver nanoparticles

Silver nanoparticles were prepared from a polyacrylonitrile (PAN)/N,N‐dimethylformamide solution of silver nitrate (0.05–0.5 wt %) with light treatment (xenon arc) to reduce Ag⁺ ions into Ag⁰. The formation of silver nanoparticles in the PAN solution and the effect of treatment time on the numbers of silver nanoparticles, their average diameter and size distribution were investigated by UV–visible spectroscopy. In addition, the average size of silver nanoparticles and their shapes in colloidal solution were determined by transmission electron microscopy images and found to be on the order of 10 nm. The resulting solution was electrospun into PAN nanofibers. An increase in the salt concentration led to decreases in the nanofiber diameter and bead numbers (determined by scanning electron microscopy images) and an increase in the crystallinity (confirmed by X‐ray diffraction patterns). A continuous rate of silver release from the nanofiber web was monitored by the atomic absorption technique. These nanofibers showed strong antibacterial activity against Pseudomonas aeruginosa. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

聚乙烯吡咯烷酮/银纳米复合纤维膜的制备及抗菌性

通过液相原位还原法(用乙醇还原硝酸银)获得了合有银纳米粒子的溶胶,从而制得聚乙烯吡咯烷酮(PVP)/银纳米粒子/乙醇纺丝液;再利用静电纺丝技术,得到了含有银纳米粒子的PVP纳米复合纤维膜.利用紫外光谱仪(UV-vis)对溶胶内银纳米粒子进行了表征,运用扫描电子显微镜(SEM)和透射电子显微镜(TEM)对纤维及其内部的纳米粒子的形貌结构和分布进行了表征,并且测试了该样品对大肠埃希菌的抗菌性能.结果表明:利用静电纺丝方法可制取PVP/银纳米粒子复合纤维膜,该膜具有抗菌性.     

A convenient approach to synthesize stable silver nanoparticles and silver/polystyrene nanocomposite particles

In this study, silver nanoparticles were prepared by the reduction of silver nitrate in SDS+ isopentanol/styrene/H₂O reverse microemulsion system using sodium citrate as reducing agent. The Ag/PS nanocomposite particles were prepared by in situ emulsion polymerization of the styrene system containing silver nanoparticles that did not separate from the reaction solution. The polymerization dynamic characteristic was studied, at the same time, silver nanparticles and the encapsulation of composite particles were characterized by Fourier‐transform‐infrared spectroscopy (FTIR), transmission electron microscopy (TEM), X‐ray diffraction (XRD) measurement, UV–vis diffuse reflectance spectroscopy, and X‐ray photoelectron spectroscopy (XPS). The results of TEM and UV–vis absorption spectra showed that well‐dispersed silver nanoparticles have a narrow size distribution. XRD showed that Ag and Ag/PS nanocomposite particles were less than 10 and 20 nm in size, which is similar to those observed by TEM. The results of XPS spectra revealed that the microemulsion system can stabilize the silver nanoparticles from aggregation and provided supporting evidence for the polystyrene encapsulated silver nanoparticle structure. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008.     

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.     

Preparation of atactic poly(vinyl alcohol)/silver composite nanofibers by electrospinning and their characterization

Poly(vinyl alcohol) (PVA)/silver composite nanofibers were successfully prepared by the electrospinning method. Water‐based colloidal silver in a PVA solution was directly mixed without any chemical or structural modifications into PVA polymer fibers to form organic–inorganic composite nanofibers. The ratio of silver colloidal solution to PVA played an important role in the formation of the PVA/silver composite nanofibers. We prepared two different atactic PVA/silver nanocomposites with number‐average degrees of polymerization of 1700 and 4000 through electrospinning with various processing parameters, such as initial polymer concentration, amount of silver colloidal solution, applied voltage, and tip‐to‐collector distance. The PVA/silver composite nanofibers were characterized by field emission scanning electron microscopy and transmission electron microscopy (TEM). TEM images showed that silver nanoparticles with an average diameter of 30–50 nm were obtained and were well distributed in the PVA nanofibers. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Preparation and properties of electrospun poly(vinyl alcohol)/silver fiber web as wound dressings

A novel wound dressing material was prepared by electrospinning poly(vinyl alcohol) (PVA)/AgNO₃ aqueous solution into nonwoven webs and then treating the webs by heat or UV radiation. Through SEM, TEM, and XPS analyses, it was observed that the silver (Ag) nanoparticles were generated and existed in the near surface of the electrospun nanofibers. It was found that heat treatment as well as UV radiation reduced the Ag⁺⁺⁺ ions in the electrospun PVA/AgNO₃ fiber web into the Ag nanoparticles. Also the heat treatment improved the crystallinity of the electrospun PVA fiber web and so it made the web unsolved in moisture environment. Therefore, it was concluded that the only heat treated electrospun PVA/AgNO₃ fiber web was a good material as wound dressings because it had structural stability in moisture environment as well as excellent antimicrobial ability and, quick and continuous release of the effectiveness. POLYM. ENG. SCI., 47:43–49, 2007. © 2006 Society of Plastics Engineers     

Preparation and properties of electrospun PAN/Fe3O4 magnetic nanofibers

Polyacrylonitrile (PAN)/Fe₃O₄ composite nanofibers were prepared via the electrospinning of the PAN spinning solutions with magnetite Fe₃O₄ nanoparticles. The experimental results showed that the morphology and diameter of the nanofibers strongly depended upon concentrations of PAN and salt additives in the spinning solutions. A suitable PAN concentration and LiCl additives could effectively prevent the occurrence of beads in the electrospinning process and affected the diameters of the electrospun nanofibers. The breaking strength and breaking strain decreased when the magnetite Fe₃O₄ nanoparticles were incorporated. The prepared PAN/Fe₃O₄ nanofibers were superparamagnetic at room temperature. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Fabrication and characterization of magnetic cobalt ferrite/polyacrylonitrile and cobalt ferrite/carbon nanofibers by electrospinning

An electrospinning process was used to fabricate cobalt ferrite (CoFe₂O₄)-embedded polyacrylonitrile (PAN) nanofibers. Oleic acid-modified CoFe₂O₄ nanoparticles were dispersed in the PAN before spinning. The surface morphologies and structures of the nanofibers were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM and TEM observation showed that the average diameter of the CoFe₂O₄/PAN nanofibers was 110 nm, and the magnetic CoFe₂O₄ nanoparticles were embedded in the PAN nanofibers. X-ray photoelectron spectroscopy was used to characterize the CoFe₂O₄/PAN and CoFe₂O₄/carbon nanofibers. Fiber magnetic properties were measured by vibrating sample magnetometry, showing that the saturation magnetization of the CoFe₂O₄/PAN nanofibers was 45 emu/g and that the fibers demonstrated superparamagnetic behavior.     

Fabrication of Au/PVP nanofiber composites by electrospinning

Gold nanoparticles prepared by trisodium citrate reduction of HAuCl₄ in poly(vinylpyrrolidone) (PVP) ethanol solution were dispersed into PVP nanofibers by electrospinning. The optical property of Au nanoparticles before and after electrospinning was measured by UV‐Vis. The morphology and distribution of gold nanoparticles in PVP nanofibers were observed by transmission electron microscopy (TEM). The influence of the amount of Au added to and the concentration of PVP in electrospinning solution over the morphology of Au/PVP nanofibers were studied. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Antibacterial activity of photocatalytic electrospun titania nanofiber mats and solution-blown soy protein nanofiber mats decorated with silver nanoparticles

Highly porous photocatalytic titania nanoparticle decorated nanofibers were fabricated by electrospinning nylon 6 nanofibers onto flexible substrates and electrospraying TiO₂ nanoparticles onto them. Film morphology and crystalline phase were measured by SEM and XRD. The titania films showed excellent photokilling capabilities against E. coli colonies and photodegradation of methylene blue under moderately weak UV exposure (≤ 0.6 mW/cm² on a 15-cm illumination distance). In addition, solution blowing was used to form soy protein-containing nanofibers which were decorated with silver nanoparticles. These nanofibers demonstrated significant antibacterial activity against E. coli colonies without exposure to UV light. The nano-textured materials developed in this work can find economically viable applications in water purification technology and in biotechnology. The two methods of nanofiber production employed in this work differ in their rate with electrospinning being much slower than the solution blowing. The electrospun nanofiber mats are denser than the solution-blown ones due to a smaller inter-fiber pore size. The antibacterial activity of the two materials produced (electrospun titania nanoparticle decorated nanofibers and silver-nanoparticle-decorated solution-blown nanofibers) are complimentary, as the materials can be effective with and without UV light, respectively.     

Fabrication and characterization of chitosan/poly(vinyl alcohol) electrospun nanofibrous membranes containing silver nanoparticles for antibacterial water filtration

Electrospun nanofibrous membranes (ENMs) were fabricated based on chitosan/poly(vinyl alcohol) (CS/PVA) with a 70/30 mass ratio containing silver nanoparticles (AgNPs) via the electrospinning method. AgNPs were produced on the surface of CS/PVA nanofibers by adding AgNO₃ to a CS/PVA blend solution as a silver rendering component. The presence of AgNPs in the polymer blend solution was detected by UV spectrophotometry. The morphology of nanofibers before and after cross-linking with glutaraldehyde was investigated by the field emission scanning electron microscopy. The formation and size distribution of AgNPs onto the surface of nanofibers were observed by transmission electron microscopy and confirmed by energy dispersing X-ray spectroscopy. As-spun and cross-linked CS/PVA nanofibers revealed a smooth surface with diameters ranging from 58 to 73 nm and 95 to 109 nm, respectively. The effect of AgNP formation on the chemical structure of nanofibers was explored by Fourier transform infrared spectroscopy. Static and dynamic antibacterial filtration efficiencies of CS/PVA ENMs, containing differing amounts of AgNO₃, have been tested against Escherichia coli, a gram negative bacterium. The antibacterial assessment results exhibited a significant increase in both static and dynamic antibacterial filtration efficiencies of the prepared CS/PVA ENMs by addition of AgNO₃ as a bactericidal agent.     

Ag/AgCl coated polyacrylonitrile nanofiber membranes: Synthesis and photocatalytic properties

A membrane based photocatalyst consisting of Ag/AgCl coated PAN nanofibers was synthesized in large quantities by electrospinning technique combining electroless plating method and subsequent in situ oxidation strategy. Electrospinning was firstly used to fabricate PAN/AgNO₃ composite nanofibers. After reduction, Ag nanoparticles dispersed along the nanofibers act as seeds in the following metal electroless plating step for the growth of continuous Ag shell. Then an in situ oxidation reaction between Ag shells and FeCl₃ solution was carried on to prepare Ag/AgCl coated PAN nanofiber membranes. The as-prepared materials exhibited excellent photocatalytic activity under visible-light, long-term stability, flexibility, as well as easy separation from the liquid. The present work can open a new and effective route for preparing high-performance membrane based photocatalysts for practical application.     

Microwave‐assisted rapid fabrication of antibacterial polyacrylonitrile microfibers/nanofibers via nitrile click chemistry and electrospinning

Postmodified polyacrylonitrile (PAN) microfibers/nanofibers with durable antibacterial performance was fabricated by a rapid and green method of microwave irradiation and electrospinning technologies. The fibers were endowed with antibacterial activity because of silver ions, which were embedded into PAN by nitrile click chemistry with microwave irradiation; they were then electrospun into neat and smooth microfibers/nanofibers. The obtained microfibers/nanofibers were tested against Staphylococcus aureus and exhibited powerful and long‐lasting antibacterial properties. The production of endurable antibacterial materials could effectively prevent the spread of microbes and beautify the living environment. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45490.     

Preparation and characterization of electrospun poly(ε‐caprolactone)/poly(vinyl pyrrolidone) nanofiber composites containing silver particles

A nanofiber membrane composed of poly(ε‐caprolactone) (PCL), poly(vinyl pyrrolidone) (PVP), and silver nanoparticles was prepared via electrospinning technique. The morphology and structure of the PCL/PVP/Ag nanofibers composite were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR), X‐ray diffraction (XRD), and X‐ray photoelectron spectroscopy (XPS). The SEM images showed that various composites of PCL/PVP/Ag could be electrospun to yield continuous and uniform nanofibers. FTIR spectra indicated that the molecular interactions between PCL and PVP are weak. The hydrophilicity, mechanical property, and swelling behavior of the as‐spun composites can be manipulated by altering the blend ratio of PCL/PVP. XRD patterns and XPS spectra showed that the Ag nanoparticles were dispersed in the PCL/PVP nanofiber composites; and the Ag nanoparticles endowed the PCL/PVP/Ag composite with antibacterial activities. The obtained PCL/PVP/Ag nanofiber composites with the morphology similar to that of native extracellular matrix have the potential to create a moist environment and to kill bacteria, which make it possible to be used for wound dressing application. POLYM. COMPOS., 37:2847–2854, 2016. © 2015 Society of Plastics Engineers     

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.     

In situ fabrication of polyaniline‐silver nanocomposites using soft template of sodium alginate

Polyaniline (PANI)‐Ag nanocomposites were synthesized by in situ chemical polymerization approach using ammonium persulfate and silver nitrate as oxidant. Characterizations of nanocomposites were done by ultraviolet–visible ( UV–vis), Fourier transform infrared (FTIR), X‐ray diffraction (XRD), scanning electron microscopy, and transmission electron microscopy (TEM). UV–vis, XRD and FTIR analysis established the formation of PANI/Ag nanocomposites and face‐centered‐cubic phase of silver. PANInanofibers were of average diameter ～ 30 nm and several micrometers in length. Morphological analysis showed that the spherical‐shaped silver nanoparticles decorate the surface of PANI nanofibers. Silver nanoparticles of average diameter ～ 5–10 nm were observed on the TEM images for the PANI‐Ag nanocomposites. Such type of PANI‐Ag nanocomposites can be used as bistable switches as well as memory devices. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013