‘Green’ synthesis and optical properties of silver–chitosan complexes and nanocomposites

Silver nanoparticles were synthesized in a chitosan biopolymer by an in situ ‘green’ chemical procedure, using d-glucose as the reducing agent. The reaction intermediates (silver–chitosan complexes) as well as the obtained nanocomposites were investigated using transmission electron microscopy, UV–vis, FTIR and photoluminescence spectroscopy. The theoretical analysis of the UV–vis absorption of the Ag–chitosan complexes suggested that the significant contribution to the complex spectrum arises from clusters of silver containing 4–9 atoms. The absorption spectrum of the nanocomposite exhibited a strong surface plasmon resonance band at 406 nm. The photoluminescence behavior of the pure chitosan, the silver–chitosan complexes and the nanocomposites were discussed in terms of morphology and silver weight content.     

A facile synthesis of a novel three‐phase nanocomposite: Single‐wall carbon nanotube/silver nanohybrid fibers embedded in sulfonated polyaniline

A three‐phase water‐soluble nanocomposite of single wall carbon nanotube/silver nanoparticle hybrid fibers embedded in sulfonated polyaniline has been synthesized by a simple chemical solution mixing process. The nanocomposite has been characterized by high resolution electron microscopy, X‐ray diffractometry, FTIR spectroscopy, Raman spectroscopy, and thermogravimetric analysis. Optical and electrical characteristics of the nanocomposite have been determined by UV–vis absorption spectroscopy, photoluminescence spectroscopy, and four‐probe electrical conductivity measurement. A surface plasmon absorption band obtained around 460 nm indicates the presence of silver nanoparticles in the composite. The optical band gap calculation for sulfonated polyaniline vis‐a‐vis the nanocomposite supported the conductivity measurement. Over 1300 times increase in DC electrical conductivity has been observed for the three‐phase nanocomposite, with a filler loading of 20 wt %, at 306 K. This observation could be explained by Mott's variable range hopping model considering a three‐dimensional conduction. Such a nanocomposite has immense potential for use as a cathode material in lithium‐ion batteries and supercapacitors. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41692.     

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.     

Hollow mesoporous silica spheres supported Ag and Ag–Au catalyzed reduction of 4-nitrobenzo-15-crown

Hollow mesoporous silica (HMS) spheres of size within the range 120–220 nm have been prepared using propanol–water solvent as template and cetyltrimethylammonium bromide (CTAB) as stabilizer. HMS supported silver and silver–gold catalysts were prepared by impregnating metal nanoparticles on HMS and were characterized by ultraviolet–visible spectroscopy (UV–vis), dynamic light scattering (DLS), optical microscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), inductive coupled plasma optical emission spectroscopy (ICP-OES) and N₂ adsorption–desorption. The reduction of 4-nitrobenzo-15-crown (4-NB-15-C) was compared using HMS supported silver and silver–gold nanocatalysts varying experimental parameters. Bimetallic Ag–Au/HMS nanocatalysts was found to be more active than monometallic Ag/HMS nanocatalyst.     

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     

Enhancement of pervaporation performance of composite membranes through in situ generation of silver nanoparticles in poly(vinyl alcohol) matrix

Composite membranes were prepared from an aqueous solution of poly(vinyl alcohol) (PVA) and silver sulphate. The silver nanoparticles were generated in situ before crosslinking PVA matrix by reduction of silver ions using sodium borohydride. Physico‐chemical properties of the resulting composite membranes were studied using Fourier transform infrared spectroscopy (FTIR), UV–vis spectroscopy (UV–vis), thermogravimetric analysis (TGA), Wide‐angle X‐ray diffraction (WAXD), scanning electron microscopy (SEM), and universal testing machine (UTM). The UV–vis spectrum shows a single peak at 410 nm due to surface plasmon absorption of silver nanoparticles. This surely specified that silver nanoparticles are generated in PVA matrix. The membranes were under go pervaporation (PV) for separation of water from isopropanol at different temperatures. The results indicated that hydrophilicity and amorphous nature of the membranes were increased with increasing silver nanoparticles in PVA matrix. The swelling and separation performance of the membranes were studied. Both permeation flux and separation factor were increased with increasing silver nanoparticles in PVA matrix. The results showed that the membrane containing 2.5 mass% of Ag salt exhibited excellent PV performance. The values of total flux and flux of water are almost closed to each other, indicating that membranes could be effectively used to break the azeotropic point of water‐isopropanol. The long‐term test was performed at room temperature and ascertained that membranes were durable up to 30 days for the dehydration of IPA. On the basis of the estimate Arrhenius activation energy values, the efficiency of the membranes was discussed. The calculated ΔH_s values are negative for all the membranes, indicating that Longmuir's mode of sorption is predominant. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41248.     

Synthesis and characterization of hydrogel‐silver nanoparticle‐curcumin composites for wound dressing and antibacterial application

Hydrogel silver nanocomposites are found to be excellent materials for antibacterial applications. To enhance their applicability novel hydrogel‐silver nanoparticle‐curcumin composites have been developed. For developing, these composites, the hydrogel matrices are synthesized first by polymerizing acrylamide in the presence of poly(vinyl sulfonic acid sodium salt) and a trifunctional crosslinker (2,4,6‐triallyloxy 1,3,5‐triazine, TA) using redox initiating system (ammonium persulphate/TMEDA). Silver nanoparticles are generated throughout the hydrogel networks using in situ method by incorporating the silver ions and subsequent reduction with sodium borohydride. Curcumin loading into hydrogel‐silver nanoparticles composite is achieved by diffusion mechanism. A series of hydrogel‐silver nanoparticle‐curcumin composites are developed and are characterized by using Fourier transform infrared (FTIR) and UV–visible (UV–vis) spectroscopy, X‐ray diffraction, thermal analyses, as well as scanning and transmission electron microscopic (SEM/TEM) methods. An interesting arrangement of silver nanoparticles i.e., a shining sun shape (ball) (～ 5 nm) with apparent smaller grown nanoparticles (～ 1 nm) is observed by TEM. The curcumin loading and release characteristics are performed for various hydrogel composite systems. A comparative antimicrobial study is performed for hydrogel‐silver nanocomposites and hydrogel‐silver nanoparticle‐curcumin composites. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Synthesis,conductivity, and electromagnetic wave absorption properties of chiral poly Schiff bases and their silver complexes

Four chiral poly Schiff bases were synthesized via polycondensation between l‐ lysine and p‐benzoquinone, 1,4‐naphthoquinone, dibenzoyl, and 2,3‐butanedione, respectively. Subsequently, the silver coordination polymers of the chiral poly Schiff base were prepared upon silver ions coordinating with the chiral poly Schiff bases. The structures of the polymers were characterized with IR, UV‐vis, GPC, elemental analysis, and optical activity analysis. The properties of polymers were studied through conductivity testing and electromagnetic parameter testing. The results show that they own good electrical conductvities, and the electrical conductivity of chiral poly‐(l‐ lysine(2,3‐butanedione)) Schiff base silver complex can reach 3.7 × 10² S/cm. The electromagnetic wave absorption properties of four silver complexes were calculated using transmission line theory, the maximum reflection loss of chiral poly‐(l‐ lysine(p‐benzoquinone)) Schiff base silver complex can reach ?45.9 dB at a thickness of 5 mm, while that of achiral poly‐(dl ‐lysine(p‐benzoquinone)) Schiff base silver complex is ?20.1 dB at a thickness of 5 mm. The enhanced microwave absorbing properties were attributed to the chiral feature. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42498.     

Preparation of AgNPs/PS composite via reverse microemulsion polymerization

Silver nanoparticles (AgNPs) were synthesized in reverse microemulsions using silver nitrate as silver source, hydrazine hydrate as reducing agent, n‐heptane as oil phase, cetyl trimethyl ammonium bromide (CTAB) as surfactant, and isoamyl alcohol as cosurfactant. A uniform silver nanoparticles/polystyrene (AgNPs/PS) composite was further prepared by a reverse microemulsion polymerization method. The morphologies and structures of the AgNPs and the AgNPs/PS composite were characterized by UV‐visible spectroscopy (UV–vis), X‐ray diffraction (XRD), fourier transform infrared spectra (FTIR), and transmission electron microscopy (TEM). Furthermore, the molecular weight of the AgNPs/PS composite was measured by gel permeation chromatography (GPC), and the thermal stability of the AgNPs/PS composite was determined by thermal gravimetric (TG) analysis. Results show that the AgNPs have a particle size of 3–10 nm, and are almost spherical, uniform, and monodisperse both in a AgNPs colloid and in the AgNPs/PS composite. There are no characteristic peaks of silver oxide in the synthetic AgNPs and AgNPs/PS composite. The AgNPs/PS composite has a better thermal stability and a higher molecular weight than virgin PS. POLYM. COMPOS., 35:1325–1329, 2014. © 2013 Society of Plastics Engineers     

Preparation and antibacterial effects of PVA‐PVP hydrogels containing silver nanoparticles

The poly(vinyl alcohol)/poly(N‐vinyl pyrrolidone) (PVA–PVP) hydrogels containing silver nanoparticles were prepared by repeated freezing–thawing treatment. The silver content in the solid composition was in the range of 0.1–1.0 wt %, the silver particle size was from 20 to 100 nm, and the weight ratio of PVA to PVP was 70 : 30. The influence of silver nanoparticles on the properties of PVA–PVP matrix was investigated by differential scanning calorimeter, infrared spectroscopy and UV–vis spectroscopy, using PVA–PVP films containing silver particles as a model. The morphology of freeze‐dried PVA–PVP hydrogel matrix and dispersion of the silver nanoparticles in the matrix was examined by scanning electron microscopy. It was found that a three‐dimensional structure was formed during the process of freezing–thawing treatment and no serious aggregation of the silver nanoparticles occurred. Water absorption properties, release of silver ions from the hydrogels and the antibacterial effects of the hydrogels against Escherichia coli and Staphylococcus aureus were examined too. It was proved that the nanosilver‐containing hydrogels had an excellent antibacterial ability. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 125–133, 2007     

Novel simple solvent-less preparation,characterization and degradation of the cationic dye over holmium oxide ceramic nanostructures

Pure holmium oxide ceramic nanostructures were prepared via a new simple approach. Nanostructures were synthesized by heat treatment in air at 600 °C for 5 h, utilizing [Ho L(NO₃)₂]NO₃ (L=bis-(2-hydroxy-1-naphthaldehyde)-butanediamine Schiff base ligand), as precursor, which was prepared via a solvent-free solid–solid reaction from different molar ratios of holmium nitrate and Schiff base ligand. The as-prepared nanostructures were characterized by field emission scanning electron microscopy (FESEM), thermo-gravimetric analysis (TGA), X-ray diffraction (XRD), energy dispersive X-ray microanalysis (EDX), transmission electron microscopy (TEM), UV–vis diffuse reflectance spectroscopy and Fourier transform infrared (FT-IR) spectroscopy. It was found that the calcination temperature and molar ratio of holmium nitrate and Schiff base ligand have significant and key effect on the morphology and particle size of the holmium oxide. To investigate the catalytic properties of as-obtained holmium oxide nanostructures, the photocatalytic degradation of rhodamine B as cationic dye under ultraviolet light irradiation was performed.     

Synthesis of cuprous oxide using sodium borohydride under microwave irradiation and catalytic effects

Cuprous oxide nanoparticles were synthesized under microwave irradiation for 15 min to use as a catalyst. The product was confirmed by X-ray diffraction and transmission electron microscopy. The catalytic effect of cuprous oxide nanoparticles was investigated for the reduction of 4-nitrophenol to produce 4-aminophenol in the presence of NaBH₄. The above product was confirmed by UV–vis spectroscopy and liquid chromatography–mass spectroscopy.     

Enhanced surface morphology and transport property of poly(N‐vinylcarbazole)/gold nanocomposite Langmuir–Schaefer films

A composite of poly(N‐vinylcarbazole) (PVK) containing gold nanoparticles (GNPs) was synthesized via simple solid‐state in situ bulk polymerization of N‐vinylcarbazole in the presence of GNPs at a high temperature. Both PVK and PVK–GNP composites were characterized by Fourier transform infrared (FTIR) and UV–vis spectroscopy. The surface morphology of the composites was studied by scanning electron microscopy (SEM), energy‐dispersive X‐ray spectroscopy, and transmission electron microscopy (TEM). Thermal stability was identified via thermogravimetric analysis. The composites were fabricated into films using the Langmuir–Schaefer process. The enhancement in the characteristics of room temperature I–V, pressure–area isotherms, and photoelectrochemical behaviors was observed in the composite films. Results suggest that a charge transfer process occurs across the hybrid at the interface of the PVK–GNP composites. POLYM. COMPOS., 2011. © 2011 Society of Plastics Engineers     

Plant mediated green synthesis and antibacterial activity of silver nanoparticles using Crataegus douglasii fruit extract

In this study, silver nanoparticles were synthesized using the Crataegus douglasii fruit extract as a reducing agent. The reaction process was monitored by UV–vis spectroscopy. Further characterization was carried out using scanning electron microscopy (SEM). To optimize the biosynthesis of silver nanoparticles, the effect of process variables such as extract concentrations, mixing ratio of the reactants, time and pH were also investigated. The SEM images showed silver nanoparticles with 29.28 nm size and nearly spherical shape at 24 h interaction time. The antibacterial activity of the synthesized silver nanoparticles was confirmed against Staphylococcus aureus and Escherichia coli.     

Enzymatic synthesis of polyphenols with longer conjugation lengths

Polyphenols containing Schiff base pendent groups, poly(4-[benzylidene-amino]-phenol) (PBP), and poly(4-[(anthracen-9-ylmethylene)-amino]-phenol) (PAP) have been synthesized through the combination of Schiff base reaction and enzymatic polymerization using horseradish peroxidase (HRP) as catalyst. The polymers were characterized by GPC, FTIR, ¹H NMR, and UV spectroscopy. It shows that PBP and PAP are composed of polyphenol main chains bearing Schiff base pendent side groups. The PBP exhibits better solubility than PAP in some common solvents. The PAP has a large red-shift of 86 nm compared with polyphenols, indicating the Schiff base pendent groups remarkably increase the conjugation lengths of polyphenols.     

Preparation and characterization of smart hydrogel nanocomposites sensitive to oxidation–reduction

Honeycomb-patterned hydrogel films sensitive to environmental oxidation–reduction supporting nanoparticle by adsorption were fabricated through the photopolymerization of ruthenium(4-vinyl-4′-methyl-2,2′-bipyridine)bis(2,2′-bipyridine)bis(hexaflurophosphate) and N-isopropylacrylamide. Nanoparticle adsorption by the hydrogel film was controlled by the dynamic changes in the surface morphology of the film in relation to environmental oxidation–reduction, which induces change of the oxidized and reduced states of ruthenium ion included in the hydrogel. For the adsorption of nanoparticles in the patterned hydrogel film, silver nanoparticles were immobilized in the hydrogel surface. Adsorptivity was obtained through measuring the released concentration of the silver nanoparticles using UV–vis spectroscopy in an aqueous solution. Desorption of Ag nanoparticles from the hydrogel surface was found to be larger in the oxidizing solution than in the reducing solution.     

Shape control synthesis of polymeric hybrid nanoparticles via surface‐initiated atom‐transfer radical polymerization

Polymeric hybrid nanoparticles were synthesized via surface‐initiated atom‐transfer radical polymerization (SI‐ATRP) method on the surface of gold nanoparticles in cyclohexanone. Tetraoctyl ammonium bromide (TOAB) as a phase transfer agent was used to transfer the gold nanoparticles into cyclohexanone, which will be replaced by disulfide initiator on the surface of gold nanoparticles. Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and UV–vis spectroscopy were utilized to characterize the product to make sure the experiment had been conducted. The results showed that the polymeric gold hybrid nanoparticles with different structures could be controlled by adjusting the ratio of initiator and gold nanoparticles in ATRP. If the ratio is very little, asymmetric polystyrene–gold hybrid nanoparticles were synthesized, and a single gold nanoparticle was attached with a polystyrene sphere. If the ratio becomes larger, core–shell polystyrene–gold nanocomposite particles were obtained resulting in gold nanoparticle encapsulated by a uniform polymer shell. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43584.     

Cooperative catalytic activity of cyclodextrin and Ag nanoparticles immobilized on spherical polyelectrolyte brushes

Spherical polyelectrolyte brushes (SPB) loaded with silver nanoparticles (Ag‐NP) were synthesized, and they were characterized in aqueous solution using TEM, ICP‐AES and UV‐vis spectroscopy. While the size distribution of the Ag‐NP synthesized at a given temperature is quite uniform this distribution varies with change in synthesis temperature. The Ag‐NP have a strong catalytic effect on the reduction of 4‐nitrophenol to 4‐aminophenol by NaBH4. The addition of α‐cyclodextrin (α‐CD) further accelerates this 4‐nitrophenol reduction and modifies the associated activation parameters. This is attributed to α‐CD complexing 4‐nitrophenol in the vicinity of the Ag‐NP surface and thereby aiding the catalysis. © 2014 American Institute of Chemical Engineers AIChE J, 60: 1977–1982, 2014     

Antimicrobial Polychelates: Synthesis and Characterization of Transition Metal Chelated Barbituric Acid–Formaldehyde Resin

A monomeric Schiff base was prepared by the condensation reaction of salicylaldehyde and semicarbazide, which further react with formaldehyde and barbituric acid-formed polymeric Schiff base. Its metal polychelates were then formed with Mn(II), Co(II), Ni(II), Cu(II), and Zn(II). All the synthesized compounds were characterized by elemental analysis, magnetic moment, FTIR, ¹HNMR, and electronic spectroscopies. The elemental analysis data show the formation of 1:1 [M: L] metal polychelates. Thermogravimetric analysis was carried out to find the thermal behavior of all the synthesized polymeric compounds and thermal data revealed that all the metal polychelates are more thermally stable than their parent polymeric Schiff base. All the synthesized polymeric compounds were screened for antimicrobial activity against some clinically important microorganisms, such as Escherichia coli, Pseudomonas aeruginosa, Bacillus subtilis, Staphylococcus aureus, Staphylococcus typhi, Candida albicans, Microsporum canis, and Aspergillus niger. In vitro antimicrobial activity was determined by the Agar Well Diffusion method and the result shows that all the metal polychelates exhibited better antimicrobial activity than their parent polymeric Schiff base.     

Development of alginate-gum acacia-Ag0 nanocomposites via green process for inactivation of foodborne bacteria and impact on shelf life of black grapes (Vitis vinifera)

The main objective of this investigation is to develop sodium alginate-gum acacia-silver nanocomposite films (AGA-Ag⁰ NC) to inhibit the growth of foodborne and to extend the shelf life of food. The Ag nanoparticles were generated in sodium alginate-gum acacia (AGA) blend matrix through reduction by basil leaves (Tulasi). The formation of Ag⁰ was monitored by UV–vis spectroscopy (UV–Vis), Fourier transform infrared spectroscopy (FTIR), thermogravimetrical analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The absorption band at 420 nm in UV–vis spectrum and change in the band positions in FTIR spectrum of AGA-Ag⁰ NC compared to that of AGA corresponds to the formation of Ag nanoparticles. The XRD profile of AGA-Ag⁰ NC exhibits characteristic d-lines of Ag nanoparticles. The spherical shape of Ag nanoparticles uniformly formed throughout the films was recognized in SEM image with a size of ~ 4 ± 1 nm as observed by TEM. The water uptake and mechanical properties of the films were also studied. The AGA-Ag⁰NC films offered excellent antimicrobial activity against various foodborne bacteria and shelf life of food enhanced efficiency of the AGA-Ag⁰NC films is also tested on grape fruit (Vitus vinifera). © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47331.