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     

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     

Fabrication and characterization of silica/polypyrrole nanocomposites using silica sulfuric acid as templates

The sunflower‐like silica core‐polypyrrole (PPy) shell nanocomposites were prepared by using silica sulfuric acid as templates. The silica sulfuric acid was obtained by treating directly the silica nanoparticles with chlorosulfonic acid. The sulfonic groups (? SO₃H) on the surface of silica sulfuric acid not only offered the active sites for formation of polypyrrole particles but also acted as dopant agents in PPy. The nanostructures of sunflower‐like silica/PPy nanocomposites and hollow PPy capsules were investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The molecular structure and content of PPy were determined by Fourier transform infrared (FTIR) and thermal gravimetric analysis (TGA), respectively. The highest conductivity of nanocomposites is 2.4 S/cm. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

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     

Synthesis and characterization of nanosilica/polyacrylate composite latex

The nanosilica/polyacrylate organic–inorganic composite latex was synthesized by in‐situ emulsion polymerization of methyl methacrylate (MMA) and butyl acrylate (BA) in the presence of silica nanoparticles, which were modified by silane coupling agent. The surface properties and dispersibility of silica nanoparticles modification, chemical structure, Zeta potential, diameter distribution of the composite latex prepared, surface roughness, and thermal stability of the hybrid film formed by the composite latex were investigated by fourier transform infrared spectrometer (FTIR), transmission electron microscopy (TEM), Zeta meter, ZetaPlus apparatus (dynamic light scattering method), atomic force microscopy (AFM), and thermogravimetric analysis (TGA), respectively. After modification with silane coupling agent, silane was grafted onto the surface of silica nanoparticles to form the organic layers, which was able to efficiently prevent the silica nanoparticles from aggregating to individually homogeneous disperse in the in‐situ emulsion polymerization system and improve the compatibility of silica nanoparticles with the acrylate monomers. The nanosilica/polyacrylate organic–inorganic composite latex prepared had the properties of silica nanoparticles and pure polyacrylate latex but was not simply a combination. Strong chemical bonding tethered the silica and acrylate chains to form the core/shell structural composite latex. Consequently, the hybrid film formed by nanosilica/polyacrylate composite latex exhibited a smooth surface and better thermal properties than the pure polyacrylate film. POLYM. COMPOS. 27:282–288, 2006. © 2006 Society of Plastics Engineers     

Modification of silica nanoparticles with hydrophilic sulfonated polymers by using surface-initiated redox polymerization

Sulfonated polymer/silica hybrid nanoparticles were prepared by free radical polymerization of 2-acrylamido-2-methyl-1-propane sulfonic acid (PAMPS-g-SN) and styrene sulfonic acid sodium salt (PSSA-g-SN), initiated on the surfaces of aminopropyl-functionalized silica nanoparticles (ASN). Ce(IV) ammonium nitrate/nitric acid and sodium dodecyl sulfate were used as redox initiator and stabilizer, respectively. ASN Nanoparticles were synthesized by a covalently attached 3-aminopropyltriethoxysilane onto the surface of silica nanoparticles. Sulfonated monomers (AMPS or SSA) were then grafted onto the ASN nanoparticles, ultrasonically dispersed in water, using redox initiator system at 40?°C. ASN, PAMPS-g-SN and PSSA-g-SN nanoparticles were characterized by Fourier transform infrared (FTIR), thermogravimetry, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analyses. FTIR and TGA results indicated that both AMPS and SSA monomers were successfully grafted onto the silica nanoparticles. The grafted amounts of sulfonated polymers onto the silica nanoparticles were estimated from TGA thermograms to be 46 and 22?% for PAMPS and PSSA, respectively. From SEM and TEM micrographs, the average-diameters of the polymer-grafted silica nanoparticles were measured to be <50?nm with a (semi)spherical morphology, in which several silica nanoparticles were able to form a core with PAMPS or PSSA existing around the silica nanoparticles.     

Fabrication and characterization of carbon nanofibers with a multiple tubular porous structure via electrospinning

Carbon nanofibers with a multiple tubular porous structure were prepared via electrospinning from a polymer blend solution of polyacrylonitrile (PAN) and polylactide (PLA) followed by carbonization. The electrospun composite nanofibers underwent pre-oxidization and carbonization, which selectively eliminated PLA phases and transformed the continuous PAN phase into carbon, thereby porous structure formed in the carbon nanofibers. The morphologies of as-spun, pre-oxidized and carbonized nanofibers were studied by scanning electron microscope (SEM) and transmission electron microscopy (TEM). It was found that carbon nanofibers with an average diameter about 250 nm and a multiple tubular porous structure were obtained. The chemical changes during thermal treatment were studied by Fourier transform infrared spectrometer (FTIR), Raman spectra, differential thermal analysis (DTA) and thermogravimetric analysis (TG). The results showed that PLA phases were effectively removed and the continuous PAN phase was completely carbonized. The obtained carbon nanofibers had more disordered non-graphitized structures than non-porous nanofibers.     

Electrospinning silica/polyvinylpyrrolidone composite nanofibers

Small diameter nanofibers of silica and silica/polymer are produced by electrospinning silica/polyvinylpyrrolidone (SiO₂/PVP) mixtures composed of silica nanoparticles dispersed in polyvinylpyrrolidone solutions. By controlling various parameters, 380 ± 100 nm diameter composite nanofibers were obtained with a high silica concentration (57.14%). When the polymer concentration was low, “beads‐on‐a‐string” morphology resulted. Nanofiber morphology was affected by applied voltage and relative humidity. Tip‐to‐collector distance did not affect the nanofiber diameter or morphology, but it did affect the area and thickness of the mat. Heat treatment of the composite nanofibers at 200°C crosslinked the polymer yielding solvent‐resistant composite nanofibers, while heating at 465°C calcined and selectively removed the polymer from the composite. Crosslinking did not change the nanofiber diameter, while calcined nanofibers decreased in diameter (300 ± 90 nm) and increased in surface area to volume ratio. Nanofibers were characterized by scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40966.     

Synthesis and characterization of PVB/silica nanofibers by electrospinning process

This paper describes PVB/silica nanofibers which were fabricated by electrospinning. Although electrospinning has developed rapidly over the past few years, electrospinning nanofibers are still at a premature research stage which is a process by which polymer nanofibers can be formed when a droplet of viscoelastic polymer solution is subjected to high voltage electrostatic field. PVB/silica nanofibers were obtained when the PVB/silica precursor ratio was 15% and the average diameters ranged from 100 to 200 nm and increased with increasing solution concentration and electrospinning synthesized at 12 kV of the applied voltage. The morphologies and structures of PVB/silica nanofibers were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric analyzer (TGA), Fourier transform infrared spectrometer (FTIR), energy dispersive spectrometer (EDS).     

Synthesis and characterization of poly(γ‐methacryloxypropyltrimethoxysilane)‐grafted silica hybrid nanoparticles prepared by surface‐initiated atom transfer radical polymerization

Poly(γ‐methacryloxypropyltrimethoxysilane) (PMPTS)‐grafted silica hybrid nanoparticles were prepared by surface‐initiated atom transfer radical polymerization (SI‐ATRP). The resulting PMPTS‐grafted silica hybrid nanoparticles were characterized using Fourier transform infrared spectroscopy (FTIRS), nuclear magnetic resonance (NMR), gel permeation chromatography (GPC), X‐ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy (SEM), static water contact angle (WCA) measurement, and thermogravimetric analysis (TGA). Combined FTIRS, NMR, XPS, SEM, and TGA studies confirmed that these hybrid nanoparticles were successfully prepared by surface‐initiated ATRP. SEM and AFM studies revealed that the surfaces of the nanoparticles were rough at the nanoscale. In addition, the results of the static WCA measurements showed that the nanoparticles are of low surface energy and their surface energy reaches as low as 6.10 mN m^?1. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Preparation of monodispersed silica spheres and electrospinning of poly(vinyl alcohol)/silica composite nanofibers

In this study, monodispersed silica spheres were successfully synthesized by seed‐growth method and they can be highly dispersed in the poly(vinyl alcohol)(PVA) solution. PVA/silica composite fibers were fabricated by electrospinning the composite solutions containing different amount of silica. Further investigation showed that the size distribution of silica sphere was monodispersed and the spheres were homogeneously dispersed in the fibers individually. The composite fibers showed an uniform and continuous morphology with a average diameter of 298–345 nm. The as‐spun nanofibers were characterized by Field Emission Scanning Electron Microscope (FE‐SEM), transmission electron microscopy (TEM), X‐ray diffraction (XRD), and thermal gravimetric analysis (TGA). POLYM. COMPOS., 2011. © 2011 Society of Plastics Engineers     

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     

Development of a transparent PMMA composite reinforced with nanofibers

Core‐shell composite nanofibers with PA‐6 (Nylon‐6) as core and Poly (methyl methacrylate) (PMMA) as shell were fabricated by a coaxial electrospinning method, which were later made into nanofiber reinforced transparent composites through a hot press treatment. Morphological and structural characterizations for the composite nanofibers and the transparent composites were realized in terms of SEM, TEM, and FTIR techniques. The fiber reinforcement feature of the PA‐6 was demonstrated by the SEM photos of a composite sample fractured in liquid nitrogen. Through TGA and DSC tests, it was observed that thermal endurance and glass‐transition temperature of the nanofiber reinforced composites altered in variation with the contents of the reinforcing PA‐6. Experimental results indicated that the mechanical performance of the nanofiber reinforced transparent composites was obviously improved, and its transparency decreased a little with an increase in the PA‐6 content. As long as, however, a sacrifice of 10% in transparency was specified, an increment of more than 20% in the mechanical properties of the composites was achievable. POLYM. COMPOS., 2009. © 2008 Society of Plastics Engineers     

Preparation and characterization of pyrrole/aniline copolymer nanofibrils using the template‐synthesis method

Copolymer nanofibrils composed of pyrrole and aniline had been prepared by synthesizing the desired polymer within the pores of microporous anodic aluminum oxide (AAO) template membrane. To analyze their structure and properties, FTIR spectra were taken and thermogravimetric analysis (TGA) was applied. Also, the copolymer nanofibrils were photographed under scanning electron microscopy (SEM) and transmission electron microscopy (TEM) for microstructure analysis, and the conductivities were obtained by the four‐probe method. The result of SEM and TEM revealed that the obtained copolymer nanofibrils had uniform and well‐aligned array, and their diameter and length can be controlled by changing the aspect ratios of the AAO membrane. The result of IR spectrometry and TGA indicated that both polypyrrole and polyaniline were involved in the copolymer. The obtained nanofibrils were identified to be copolymer rather than composite. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 3002–3007, 2001     

Surface‐modified silica nanoparticles for reinforcement of PMMA

Polymethyl methacrylate (PMMA) was introduced onto the surface of silica nanoparticles by particle pretreatment using silane coupling agent (γ‐methacryloxypropyl trimethoxy silane, KH570) followed by solution polymerization. The modified silica nanoparticles were characterized by Fourier‐transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). Sedimentation tests and lipophilic degree (LD) measurements were also performed to observe the compatibility between the modified silica nanoparticles and organic solvents. Thereafter, the PMMA slices reinforced by silica‐nanoparticle were prepared by in situ bulk polymerization using modified silica nanoparticles accompanied with an initiator. The resultant polymers were characterized by UV–vis, Sclerometer, differential scanning calorimetry (DSC). The mechanical properties of the hybrid materials were measured. The results showed that the glass transition temperature, surface hardness, flexural strength as well as impact strength of the silica‐nanoparticle reinforced PMMA slices were improved. Moreover, the tensile properties of PMMA films doped with silica nanoparticles via solution blending were enhanced. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Enhancement of heavy metal ion adsorption using electrospun polyacrylonitrile nanofibers loaded with ZnO nanoparticles

This article describes the adsorption and tensile behavior of electrospun polyacrylonitrile (PAN) nanofiber mats loaded with different amounts of ZnO [0.5, 1.0, 2.0, and 5.0 wt%] nanoparticles. X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transforminfrared (FTIR) spectroscopy, and thermal gravimetric analysis (TGA) were utilized to characterize the resulting composite nanofibers. Microscopic investigations revealed that the increase in surface roughness and diameter of the electrospun PAN nanofibers was due to the addition of ZnO nanoparticles. Adsorption results indicated that the fabricated PAN/ZnO (2.0 wt%) composite nanofiber mats showed the best adsorption performance with 261% and 167% increase in adsorption capacities for Pb(II) and Cd(II) from aqueous solutions, respectively, compared to pristine PAN nanofibers. The adsorption equilibrium was reached within 60 min, and the process could be described using the nonlinear pseudo-second-order kinetic model. The adsorption isotherm study was better represented by the Langmuir model, which suggested a homogeneous distribution of the monolayer adsorptive sites on the surface of the composite nanofibers. Mechanical testing revealed that the decrease in tensile strength and elongation at breakof the PAN/ZnO composite nanofiber mats was due to the formation of some bead defects and agglomerates within the structure of the PAN nanofibers. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47209.     

Properties of osmanthus fragrance‐loaded chitosan–sodium tripolyphosphate nanoparticles delivered through cotton fabrics

Osmanthus fragrance‐loaded chitosan nanoparticles (OF‐NPs) were prepared via complex coacervation successfully. Then, the OF‐NPs were applied in the cotton fabrics directly. The microstructures of OF‐NPs were characterized by dynamic light scattering (DLS), transmission electron microscopy (TEM), Fourier transformation infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). The sustained property of the cotton fabrics treated with OF‐NPs was investigated with scanning electron microscopy (SEM) and gas chromatography‐mass spectrometry (GC‐MS). The common OF was also treated on fabrics for the parallel comparison. TEM and DLS displayed that the spherical OF‐NPs kept about 130 nm and dispersed evenly. FTIR confirmed that OF had been interacted with chitosan via the hydrogen bonds. TGA demonstrated that the thermal stability of OF‐NPs had been improved in contrast to OF and the loading content of OF was as high as 12.05%. SEM and GC‐MS displayed that the cotton fabrics treated by OF‐NPs had an excellent washing resistance. Overall, nanoencapsulation with CS‐TPP will provide an excellent method for releasing fragrance. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Direct grafting of ε‐caprolactone on solid core/mesoporous shell silica spheres by surface‐initiated ring‐opening polymerization

Poly(?‐caprolactone) (PCL) was formed on Solid core/mesoporous shell (SCMS) silica surface by surface‐initiated ring‐opening polymerization (SI‐ROP). The SI‐ROP of ?‐caprolactone was achieved by heating a mixture of SCMS silica, ?‐caprolactone and the tin(II) 2‐ethylhexanoate [Sn(Oct)₂] in a anhydrous toluene for 20 h at different temperatures viz. 40, 60, and 80°C. The PCL grafted SCMS silica was characterized by fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), X‐ray, differential scanning calorimetry and scanning electron microscopy (SEM). The FTIR spectroscopic analysis reveals the formation of ester linkage between PCL and hydroxyl terminated SCMS silica. TGA investigation shows increase in PCL content on SCMS silica surface with increase in reaction temperature. The SEM photographs clearly show the formation of PCL polymer on the SCMS silica surface without altering the spherical nature of SCMS silica. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Grafting of water‐soluble sulfonated monomers onto functionalized fumed silica nanoparticles via surface‐initiated redox polymerization in aqueous medium

Sulfonated polymer/fumed silica hybrid nanoparticles were prepared via surface‐initiated free radical polymerization of 2‐acrylamido‐2‐methyl‐1‐propane sulfonic acid (PAMPS‐g‐FSN), styrene sulfonic acid sodium salt (PSSA‐g‐FSN) and vinyl sulfonic acid sodium salt (PVSA‐g‐FSN) from the surface of aminopropyl‐functionalized fumed silica nanoparticles (AFSNs) dispersed in aqueous medium. Cerium(IV) ammonium nitrate/nitric acid and sodium dodecyl sulfate were used as redox initiator and stabilizer respectively. AFSNs were prepared by covalently attaching 3‐aminopropyltriethoxysilane onto the surface of fumed silica nanoparticles. Sulfonated monomers (AMPS, SSA or VSA) were then grafted onto the AFSNs ultrasonically dispersed in water via redox initiation at 40 °C. Structure, thermal properties, particle size and morphology of the AFSNs and PAMPS‐g‐FSN, PSSA‐g‐FSN and PVSA‐g‐FSN hybrid nanoparticles were characterized by Fourier transform infrared spectroscopy, TGA, SEM, transmission electron microscopy (TEM) and dynamic light scattering (DLS). The results indicated that the sulfonated monomers were successfully grafted onto the fumed silica nanoparticles. Grafting amounts of the sulfonated polymers onto the fumed silica nanoparticle surface were estimated from TGA thermograms to be 59%, 13% and 29% for the PAMPS, PSSA and PVSA, respectively. From SEM, TEM and DLS analysis, polymer‐grafted fumed silica nanoparticles with an average diameter smaller than 70 nm and a (semi‐) spherical shape were observed. A significant bimodal particle size distribution was observed only for the PAMPS‐g‐FSN with average diameters of 39.6 nm (84.1% per number) and 106 nm (15.9% per number). The hydrophilic sulfonated polymer/grafted fumed silica obtained from the redox graft polymerization gave a stable colloidal dispersion in acidic aqueous medium. Copyright © 2012 Society of Chemical Industry     

Slow release of levofloxacin conjugated on silica nanoparticles from poly(ɛ-caprolactone) nanofibers

Composite levofloxacin (LVF)/nanofibers have been fabricated through electrospinning. Slow release was achieved by covalently binding LVF to mesoporous silica nanoparticles (MSN) through a cleavable thioester bond and then blending the MSN into poly(?-caprolactone) (PCL) nanofibers. Conjugated LVF–MSN was characterized by FTIR, DSC, TGA, and solid-state C¹³ NMR. The structure of composite nanofibers was studied by scanning electron microscopy (SEM). Drug release profiles showed that burst release was decreased from 59% in the uniform PCL/LVF electrospun mats to 20% in the PCL/conjugated LVF–MSN mats after 1 day in phosphate buffer at 37°C, and gradual release in the latter was observed over the next 13 days. This slow release is due to the cleavable bond between LVF and MSN that can be hydrolyzed over a time and results in slow release of LVF. The results indicate that confining drug-conjugated MSN into nanofibers are effective ways to slow down the burst release of the drug.