Synthesis and characterization of a copolymer: Poly(aniline‐co‐fluoroaniline)

In the present article, we report the chemical synthesis and characterization of poly(aniline‐co‐fluoroaniline) [poly(An‐FAn)]. The copolymerization of aniline and 2‐fluoroaniline was carried out by chemical method in acidic medium. The characterization of poly(aniline‐co‐fluoroaniline) was done using FTIR, UV‐visible spectroscopy, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), scanning electron micrography (SEM), and a four‐points‐probe conductivity method. X‐ray diffraction (XRD) and SEM characterization reveal crystalline nature of doped copolymer compared to undoped copolymer. The observed decrease in the conductivity of the copolymer relative to polyaniline is attributed to the incorporation of the fluoro moieties into the polyaniline chain. The chemically synthesized copolymer shows good solubility in common organic solvents, and is, therefore, technological useful. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 81: 1460–1466, 2001     

Epoxy‐montmorillonite clay nanocomposites: Synthesis and characterization

Nanocomposites of epoxy resin with montmorillonite clay were synthesized by swelling of different proportions of the clay in a diglycidyl ether of bisphenol‐A followed by in situ polymerization with aromatic diamine as a curing agent. The montmorillonite was modified with octadecylamine and made organophilic. The organoclay was found to be intercalated easily by incorporation of the epoxy precursor and the clay galleries were simultaneously expanded. However, Na‐montmorillonite clay could not be intercalated during the mixing or through the curing process. Curing temperature was found to provide a balance between the reaction rate of the epoxy precursor and the diffusion rate of the curing agent into the clay galleries. The cure kinetics were studied by differential scanning calorimetry. The exfoliation behavior of the organoclay system was investigated by X‐ray diffraction. Thermogravimetric analysis was used to determine the thermal stability, which was correlated with the ionic exchange between the organic species and the silicate layers. The morphology of the nanocomposites was evaluated by scanning electron microscopy. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 2201–2210, 2004     

Rubber–clay nanocomposite by solution blending

Ethylene vinyl acetate rubber (45% vinyl acetate content, EVA‐45) and organomodified clay (12Me‐MMT) composites were prepared by solution blending of the rubber and the clay. A combination of X‐ray diffraction, scanning electron microscopy, and transmission electron microscopy studies showed that the composites obtained are on the nanometer scale. The measurements of the dynamic mechanical properties for different compositions over a temperature range (?100 to +100°C) showed that the storage moduli of these rubber–clay nanocomposites are higher above the glass to rubber transition temperature compared to the neat rubber. The tensile strength of the nanocomposites is about 1.6 times higher than that of the EVA‐45. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 87: 2216–2220, 2003     

Elaboration and thermal analysis of nanocomposites based on poly(methyl methacrylate‐co‐4‐vinylpyridine) and Maghnia bentonite

Nanocomposites based on an organically modified bentonite, from Maghnia Algeria (OBT) and a copolymer of methyl methacrylate with 4‐vinylpyridine (PMM4VP) synthesized in dioxan at room temperature using a neutral Ni(II)α‐benzoinoxime complex as a single component initiator, were elaborated via solution intercalation method and characterized by several techniques. X‐ray diffraction and transmission electron microscopy investigations indicate that mainly exfoliated and intercalated PMM4VP/OBT nanocomposites were elaborated and that the degree of exfoliation decreases with an increase of the OBT loading. Thermal analyses of these nanocomposites compared with their virgin copolymer confirmed a significant improvement of their thermal stability as evidenced by an increase of 28°C in their onset degradation temperatures. In addition, differential scanning calorimetry displayed an increase in the range of 12–18°C in their glass transition temperatures relative to their virgin copolymer. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Effect of different compatibilisers on nanoclay dispersion,thermal stability,and burning behavior of polypropylene–nanoclay blends

The dispersion of nanoclays in nonpolar polypropylene (PP) is difficult without the use of a small fraction (1–3%) of modified grafted PP as a compatibiliser. This work reports the effect of different graft‐modified polypropylenes on the dispersion of nanoclays in PP, and thermal stability and flammability of the blends. PP has been compounded in a Brabender compounder with a selection of modified PP polymers as compatibilisers. The grafts include maleic anhydride, N‐ethylmaleimide, diethylmaleate, diethyl‐p‐vinylbenzyl phosphonate, and acrylic acid‐2‐[(diethoxyphosphoryl)methylamino] ethyl ester. Films were cast from the blends by compression molding and the nanocomposite structures assessed using X‐ray diffraction. Thermal characterization was performed using DSC and TGA, the burning behavior was observed using limiting oxygen index measurements, and cone calorimetry where samples were exposed to 35 kW/m² external heat flux. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Photoluminescence characterization and heat treatment effect on luminescence behavior of BaTa2O6:Dy3+ phosphor

Undoped and Dy³⁺‐doped barium tantalate phosphors were synthesized by the solid‐state reaction method at 1425°C. Also, 10 mol% Dy³⁺‐doped BaTa₂O₆ was sintered between 1150 and 1425°C in order to determine temperature effect on structural and luminescence properties. Afterwards, they were characterized by XRD, SEM‐EDS and photoluminescence (PL) analyses. PL spectra exhibited the excitation peaks between 300 and 440 nm. Two typical emissions were observed at 486.2 nm (blue) and 577.7 nm (yellow) due to the ⁴F_9/2→⁶H_15/2 and ⁴F_9/2→⁶H_13/2 transitions, respectively. Emission intensities increased with increasing doping concentration of Dy³⁺ up to 10 mol% and then decreased due to the concentration quenching effect. Moreover, depending on the increase in heat treatment temperature, the intensity of emission reached maximum at 1425°C. The calculated CIE chromaticity coordinates of phosphors located in the white light region.     

Synthesis,structural characterization,and photoluminescence properties of TTB‐type PbTa2O6:Eu3+ phosphor

Undoped and Eu³⁺‐doped tetragonal tungsten bronze (TTB) PbTa₂O₆ phosphors were synthesized by using solid‐state reaction method. Synthesized samples were characterized by XRD, SEM‐EDS, and photoluminescence analyses. XRD results revealed TTB‐type crystal structure with single phase up to 10 mol% Eu³⁺ doping concentration. In SEM‐EDS analyses, elemental composition of Pb decreased with the increasing concentration of Eu³⁺. Emissions at the excitation wavelength of 398.5 nm were observed at 593.2 and 618.8 nm due to ⁵D₀→⁷F₁ transitions and ⁵D₀→⁷F₂ transitions, respectively. Emission increased with the increasing Eu³⁺ doping concentration up to 10 mol% and not observed concentration quenching.     

Synthesis and characterization of biodegradable polyethylene by graft copolymerization of starch using glucose–Ce(IV) redox system

Graft copolymerization of low‐density polyethylene (LDPE) onto starch was carried out with glucose–cerium(IV) redox initiator in an aqueous sulfuric acid medium under nitrogen atmosphere. The graft yield was influenced by various parameters like reaction time, temperature, and concentrations of acid, glucose, polyethylene (PE), starch, and initiator. A maximum graft yield of 85.66% was obtained at a temperature of 50°C and at higher concentration of starch. Effect of grafting on crystallinity, morphology, and thermal properties of modified PE has been evaluated using X‐ray diffraction, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA/DTA). Biodegradability of starch‐grafted PE has been tested applying soil‐burial test. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 3229–3239, 2006     

Chemical synthesis and characterization of polyaniline nanofiber doped with gadolinium chloride

Gadolinium Chloride (GdCl₃) has been employed as dopant to synthesize conductive polyaniline (PANI) using chemical method. The resulting products were characterized using infrared spectroscopy, UV–vis spectra, scanning electron microscope, differential thermal analyzer, and X‐ray diffraction. It was found that Gd³⁺ can interact with PANI chains and induce changes on the properties of PANI. The addition of GdCl₃ could greatly increase electrical conductivity and crystalline degree of PANI. Changes in UV–vis and FTIR spectra show that there exists interaction between gadolinium ions and PANI chain. The effect of different proportions of ammonium persulfate on the properties of PANI was also discussed. When the molar ratios of GdCl₃ to aniline is 2 : 1 and ammonium persulfate to aniline is 1 : 1, the more uniform and regular PANI nanofiber can be prepared. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 946–953, 2006     

Local structure of the MgxNixCoxCuxZnxO(x=0.2) entropy‐stabilized oxide: An EXAFS study

Entropy‐stabilized oxides (ESOs) provide an alternative route to novel materials discovery and synthesis. It is, however, a challenge to demonstrate that the constituent elements in an entropy‐stabilized crystal are homogeneously and randomly dispersed among a particular sublattice, resulting in a true solid solution with no evidence of local order or clustering. In this work, we present the application and analysis of extended X‐ray absorption fine structure (EXAFS) on the prototype ESO composition Mg_xNi_xCo_xCu_xZn_xO (x=0.2). In so doing, we can quantify the local atomic structure on an element‐by‐element basis. We conclude that local bond lengths between metal and oxygen vary around each absorbing cation, with notable distortion around the Cu–O polyhedra. By the second near neighbor (i.e., the cation‐cation pair), interatomic distances are uniform to the extent that the collected data can resolve. Crystal models that best fit the experimental scattering data include cations that are distributed randomly on an FCC sublattice with minimal positional disorder, with an interleaved FCC anion sublattice with oxygen ions displaced from the ideal locations to accommodate the distortions in the cation polyhedra. Density functional theory calculations of the ESO system yield a significant broadening in the positional distribution for the oxygen sublattice compared to that for the cation sublattice for all peaks, showing consistency with the conclusion from the experimental data that the distortion from an ideal rock salt structure occurs primarily through disorder in the oxygen sublattice.     

Surface and bulk properties improvement of HDPE by a batch plasma treatment

High‐density polyethylene (HDPE) pellets were modified via atmospheric plasma treatment using nitrogen flushing. The new application of plasma treatment was introduced in this work, namely a batch treatment on plastic pellets just prior to its feeding to the extrusion process in comparison with the conventional surface treatment of the plastic sheet. The effect of treatment time (15–120 s) on wettability, chemical, thermal, and mechanical properties of the modified HDPE were investigated and compared with the typical surface‐treated HDPE and untreated HDPE. The pellet treatment distributed well the hydrophilicity groups so that both surface and bulk properties were improved. It showed an enhancement of wettability similar to surface treatment at short treatment time (15 s). Attenuated total reflection‐Fourier transform infrared spectroscopy and X‐ray photoelectron spectroscopy revealed the presence of new chemical groups (nitrogen and oxygen up to 5 and 42 at %, respectively). In addition, crosslinked structure was also disclosed by solvent extraction (gel content of 3.5–5.5 wt % increased with treatment time) and significantly affected to decrease the crystallinity from 76% in the untreated sample to 63%. The decomposition process of the pellet treatment samples was delayed. Lastly, pellet treatment yielded advantages in remaining hydrophilicity during aging and improving mechanical properties. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43011.     

Synthesis and characterization of gelatin‐polydimethylsiloxane graft copolymers

Gelatin‐polydimethylsiloxane (PDMS) graft copolymers were prepared through the reaction between gelatin and α‐[3‐(2,3‐epoxypropoxy)propyl]‐ω‐butyl‐PDMSs. The copolymers were characterized by FTIR and ¹H‐NMR spectra. As proved by wide angle X‐ray analysis, a new characteristic crystalline peak appeared after the bonding of PDMS to gelatin chains. The microstructure and the elemental identification of gelatin and copolymers were followed through scanning electron microscope with energy dispersive spectrometer. The glass transition temperature of gelatin and copolymers were obtained by differential scanning calorimetry analysis. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Synthesis and characterization of mercury oxide unusual nanostructures by ultrasonic method

A facile direct synthesis has been done to prepare HgO nanocrystallites of different shapes. The effect of different parameters such as the presence of alkali salts or stabilizers, power of the ultrasound, time of sonicating, and the starting materials on the size, morphology and crystallinity degree of the products were studied. Scanning electron microscopy observations revealed that using of polyvinyl alcohol (PVA) or alkali salts led to different shapes of product.     

Some metal compounds in the phase of crosslinked ionic polymer—precursors for new sorbents and catalysts

A commercial crosslinked ionic polymer AV‐17 containing ? N(CH₃)₃Cl groups was used. The common compounds of Bi(III) and Al(III); Bi(III) and Cr(III); Bi(III) and Fe(III); Bi(III) and FeOOH and of three components—Bi(III), Fe(III), and Cr(III); Bi(III), FeOOH, and Cr(III) were obtained in the AV‐17 polymer phase and investigated using scanning electron microscopy, powder X‐ray diffraction, thermogravimetric analysis, and Fourier‐transform infrared spectroscopy. It was shown that metal‐containing compounds were concentrated on the surface of the polymer granules. The compounds were in the crystalline (BiOCl) or amorphous (jarosites and oxihydroxides) state. The morphology and composition of the metal‐containing ultra dispersed particles were different on the surface and in the volume of the polymer granule. Most of the metal‐containing compounds were in the form of pseudo spherical particles, but compounds containing Bi(III) and FeOOH in the volume of AV‐17 granule, were in the form of clew of nanometer fibers. Thermogravimetric analysis (in an N₂ atmosphere) in the range 24–1000°C of the metallic compounds containing polymer was also carried out. The metal‐containing polymer samples were stable up to 120°C. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Synthesis, structure analysis, and antitumor evaluation of 3,6-dimethyl-1,2,4,5-tetrazine-1,4-dicarboxamide derivatives

3,6-Dimethyl-1,2,4,5-tetrazine-1,4-dicarboxamide derivatives were synthesized, and their structures were confirmed by single-crystal X-ray diffraction. This reaction yields the 1,4-dicarboxamide derivatives rather than the 1,2-dicarboxamide derivatives. Their in vitro antitumor activities were evaluated against SGC-7901, HO-8910, MCF-7, and A-549 cells. The results showed several compounds to be endowed with cytotoxicity in the low micromolar range. One compound (IC(50) =0.57 μM) was further evaluated in vivo against an A-549 xenograft in BALB/cA nude mice; it effected 76.4% inhibition of tumor weight through intraperitoneal (i.p.) administration of 40 mgkg(-1) body weight. Moreover, its acute toxicity was evaluated, and the i.p. LD(50) value was 325 mgkg(-1) in mice.     

Preparation and characterization of ceria nanoparticles supported on poly(4‐vinyl pyridine‐co‐divinyl benzene)

Formation of ceria nanoparticles in 2% divinyl benzene (dvb) crosslinked 4‐vinyl pyridine (4vp) polymer [poly(4vp‐co‐dvb)] microspheres was investigated. The polymer was prepared by free radical suspension polymerization method. Poly(4vp‐co‐dvb)/ceria nanocomposites were prepared by reacting CeCl₃·7H₂O and NaOH in the presence of poly(4vp‐co‐dvb) at room temperature in aqueous media. The mole ratio of the metal to polymer was varied from 2.5 to 10% with an increment of 2.5. The polymer and nanocomposities were characterized by various spectrochemical methods. The coordination of nitrogen atoms of the polymer with Ce(IV) of ceria (CeO₂) has been confirmed from X‐ray photoelectron spectroscopy (XPS). The method has yielded ceria nanoparticles in an average size of 15 nm according to transmission electron microscopy. Differential scanning calorimetry, thermogravimetric analysis, X‐ray diffractometry and XPS analysis with respect to mole percentage of ceria in the composite are discussed. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 3439–3445, 2006     

Characterization of polyurethane resins by FTIR,TGA, and XRD

Fourier Transformed Infrared Spectroscopy, Thermogravimetric Analysis, and X‐ray Diffractometry have been used to investigate the rigid, semi rigid, and soft polyurethane (PU) forms, which were developed by the Group of Analytic Chemistry and Technology of Polymers ‐ USP ‐ São Carlos. The –NCO/–OH ratios were 0.6, 0.5, and 0.3% for rigid, semi rigid, and soft PUs, respectively, showing that different ratios cause differences in thermal behaviors and crystalline structures of the synthesized PU resins. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

The effect of sulfonation treatment on the structure and properties of isotactic polypropylene fibers prior to the carbonization stage

The effect of sulfonation treatment was investigated on the molecular structure and mechanical properties of isotactic polypropylene fibers extruded at a take up speed of 2500 m/min. It was found that at extensive sulfonation times, the sulfonated structure showed the characteristic features of carbonized structure as indicated by the results of the density and the X‐ray diffraction measurements. Mechanical properties of the sulfonated samples were found to be adversely affected by the sulfonation conditions. Scanning electron microscopy observations showed surface irregularities at low sulfonation times and fiber fractures at high sulfonation times. Polarized infrared spectroscopy measurements analysed by curve fitting procedure showed increasing molecular orientation of long helical chain segments represented by the IR band at 841 cm^?1 whereas amorphous structure represented by the IR band at 2723 cm^?1 showed gradual loss of orientation with the progress of sulfonation. IR bands assigned to the sulfonic acid groups formed during sulfonation treatment showed perpendicular polarization and low molecular orientation characteristics indicating the initiation and the development of crosslinking process being perpendicular to the fiber axis direction. Analysis of the equatorial X‐ray diffraction traces showed the loss of crystallinity where the paracrystalline phase disappeared faster than the crystalline α‐monoclinic phase. During the sulfonation treatment, content of amorphous phase showed gradual increase in line with decreasing crystallinity. In accordance with the loss of crystallinity, apparent crystallite sizes corresponding to the 110, 040 and 130 planes of the α‐monoclinic phase also decreased gradually with increasing sulfonation time. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Optimizing the nanofibrous morphology of electrospun poly[(butylene succinate)‐ co‐(butylene adipate)]/clay nanocomposites and revealing the effect of the fibre nano‐dimension on the attained material properties

Electrospun mats of biodegradable polymer/clay nanocomposites were prepared in order to investigate the qualitative and quantitative correlations between electrospinning‐related parameters and the fibrous morphology of the mats. A full factorial design of experiments was used for that purpose and scanning electron microscopy was employed for dimensional characterization and determination of the chosen responses. Statistical analysis revealed that solution concentration and clay loading of nanocomposite were the most important parameters affecting the morphology of the fibrous webs. This, subsequently, allowed prediction of the domain of these two parameter settings where purely fibrous morphology can be achieved and further allowed optimization of the process in the framework of response surface methodology (RSM). The structure and thermal behaviour of the nanocomposites were also characterized before and after electrospinning using X‐ray diffraction, thermogravimetric analysis and differential scanning calorimetry. A multi‐analyte platform is provided by the combination of RSM results for improving the nanofibrous quality and post‐spinning characterization for predicting the overall performance of the electrospun web. Copyright © 2011 Society of Chemical Industry     

Synthesis and characterization of calcium‐containing poly(urethane‐urea)s

A calcium salt of mono(hydroxyethoxyethyl)phthalate [Ca(HEEP)2] was synthesized by the reaction of diethylene glycol, phthalic anhydride, and calcium acetate. Four different bisureas like hexamethylene bis(ω,N‐hydroxyethylurea), tolylene 2,4‐bis(ω,N‐hydroxyethylurea), hexamethylene bis(ω,N‐hydroxypropylurea), and tolylene 2,4‐bis(ω,N‐hydroxypropylurea) were prepared by reacting ethanolamine or propanolamine with hexamethylene diisocyanate (HMDI) or tolylene 2,4‐diisocyanate (TDI). Calcium‐containing poly(urethane‐urea)s (PUUs) were synthesized by reacting HMDI or TDI with 1:1 mixtures of Ca(HEEP)2 and each of the bisureas using di‐n‐butyltin dilaurate as a catalyst. The PUUs were well characterized by Fourier transform infrared, 1H‐ and 13C‐NMR (nuclear magnetic resonance), solid‐state 13C cross‐polarization–magic angle spinning NMR, viscosity, solubility, elemental, and X‐ray diffraction studies. Thermal properties of the polymers were also studied by using thermogravimetric analysis and differential scanning calorimetry. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 3488–3496, 2003