Effect of Nano-CaCO3 on the Structure and Properties of Holocellulose-Fiber/Polypropylene Biomass Composites

The impact of nano-CaCO₃ on the structure and properties of holocellulose-fiber/polypropylene biomass composites was conducted. With different content of nano-CaCO₃, the crystallization behavior and thermal properties of holocellulose-fiber/nano-CaCO₃/polypropylene composites were investigated by X-ray diffraction, differential scanning calorimetry, polarizing microscope, and thermogravimetric analysis. The results illustrated that the structure and properties of the composites were affected greatly by the nano-CaCO₃ and the optimal content of nano-CaCO₃ was 5 wt.%. Water absorption of composites with 5 wt.% nano-CaCO₃ decreased by 21.8% and the crystallinity increased by 14% compared with samples without nano-CaCO₃. The mechanical properties of composites also kept high performance and the thermogravimetric analysis presented the enhancement of thermal stability. All results suggested that the synergistic effect of holocellulose-fiber and nano-CaCO₃ developed a high mechanical property and low-water-absorption holocellulose-fiber/nano-CaCO₃/polypropylene ternary composites.     

Mechanical properties and fracture morphology of Al(OH)3/polypropylene composites modified by PP grafting with acrylic acid

Al(OH)₃/polypropylene (PP) composites modified by polypropylene grafted with acrylic acid (FPP) were prepared by melt extrusion. Effect of PP grafting with acrylic acid on mechanical properties and fracture morphology of Al(OH)₃/polypropylene composites were investigated. Although incorporation of Al(OH)₃ reduced the mechanical properties of PP, addition of FPP increased the mechanical properties of Al(OH)₃/PP composites. It is suggested that addition of FPP improve the dispersion of Al(OH)₃ and the interfacial interaction between filler and matrix. Mechanical properties of Al(OH)₃/FPP/PP composites depend on the grafting rate and the content of FPP. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 2617–2623, 2001     

Synthesis and characterization of alkali‐soluble photosensitive polysiloxane urethane acrylate

A new negative temperature coefficient of resistor (NTCR) thermistors based on nitrile butadiene rubber/magnetite (NBR/Fe₃O₄) nanocomposites were successfully fabricated by conventional roll milling technique. X‐ray diffraction and transmission (TEM) analysis showed that the product is mainly magnetite nanoparticles with diameter of 10‐13 nm. The microstructure of (NBR/Fe₃O₄) nanocomposites were examined by scanning electron microscopy (SEM) and FTIR spectroscopy. The dispersion of magnetite nanoparticles in the NBR rubber matrix and interfacial bonding between them were rather good. The thermal stability of nanocomposites was also obviously improved with the inclusion of the magnetite nanoparticles. The thermal conductivity, thermal diffusivity and specific heat of nanocomposites were investigated. The electrical conductivity of the NBR/Fe₃O₄ increases with the rise in temperature exhibiting a typical negative temperature coefficient of resistance (NTCR) behavior like a semiconductor. The nature of the temperature variation of electrical conductivity and values of activation and hopping energy, suggest that the transport conduction process is controlled by hopping mechanism. Values of characteristics parameters of the thermistors like thermistor constant, thermistor sensitivity and thermistor stability is quite good for practical application as NTCR devices at high temperature. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Magnetic core-bilayer shell nanoparticle: A novel vehicle for entrapmentof poorly water-soluble drugs

We are herein reporting a synthesis of indomethacin-loaded bilayer-surface magnetite nanoparticles and their releasing behavior. The particles were first stabilized with oleic acid as a primary surfactant, followed by poly(ethylene glycol) methyl ether-poly(?-caprolactone) (mPEG-PCL) amphiphilic block copolymer as a secondary surfactant to form nanoparticles with hydrophobic inner shell and hydrophilic corona. mPEG-PCL copolymers with systematically varied molecular weights of each block (2000-2000, 2000-10,000, 5000-5000 and 5000-10,000 g/mol, respectively) were synthesized via a ring-opening polymerization of ?-caprolactone using mPEG as a macroinitiator. The particles were 9 nm in diameter and exhibited superparamagnetic behavior at room temperature with saturation magnetization (M_s) about 35 emu/g magnetite. Percent of magnetite and the copolymers in the complexes were determined via thermogravimetric analysis (TGA). The effect of mPEG and PCL block lengths in the copolymer-magnetite complex on the properties of the particles, e.g. particle size, magnetic properties, stability in water, drug entrapping and loading efficiency and its releasing behavior were investigated. This novel magnetic nanocomplex might be suitable for use as an efficient drug delivery vehicle with tunable drug-released properties.     

α‐Amylase immobilized by Fe3O4/poly(styrene‐co‐maleic anhydride) magnetic composite microspheres: Preparation and characterization

Fe₃O₄/poly(styrene‐co‐maleic anhydride) core–shell composite microspheres, suitable for binding enzymes, were prepared using magnetite particles as seeds by copolymerization of styrene and maleic anhydride. The magnetite particles were encapsulated by polyethylene glycol, which improved the affinity between the magnetite particles and the monomers, thus showing that the size of the microspheres, the amount of the surface anhydrides, and the magnetite content in the composite are highly dependent on magnetite particles, comonomer ratio, and dispersion medium used in the polymerization. The composite microspheres, having 0.08–0.8 μm diameter and containing 100–800 μg magnetite/g microspheres and 0–18 mmol surface‐anhydride groups/g microsphere, were obtained. Free α‐amylase was immobilized on the microspheres containing reactive surface‐anhydride groups by covalent binding. The effects of immobilization on the properties of the immobilized α‐amylase [magnetic immobilized enzyme (MIE)] were studied. The activity of MIE and protein binding capacity reached 113,800 U and 544.3 mg/g dry microspheres, respectively. The activity recovery was 47.2%. The MIE had higher optimum temperature and pH compared with those of free α‐amylase and showed excellent thermal, storage, pH, and operational stability. Furthermore, it can be easily separated in a magnetic field and reused repeatedly. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 95: 328–335, 2005     

Morphology and properties of highly filled iPP/TiO2 nanocomposites

Nanocomposites based on isotactic polypropylene (iPP) and titanium dioxide (TiO₂) nanoparticle containing 1–15 vol% (4.6–45.5 wt%) of the nanoparticle were prepared by the melt blending process. The effect of an anhydride‐modified polypropylene as a compatibilizer on dispersion of TiO₂ nanoparticles was assessed using SEM. TGA and DSC analysis were performed to study the thermal properties of the nanocomposites. Crystalline structures of iPP in the presence of TiO₂ were analyzed by XRD. Mechanical properties of the nanoparticles were measured and a micromechanical analysis was applied to quantify interface interaction between the polymer and particle. SEM results revealed improvement of TiO₂ particle dispersion by adding the compatibilizer. It was shown that the thermal stability and crystalline structure of the nanocomposite are significantly affected by the state of particle dispersion. TiO₂ nanoparticles were shown to be strong β‐nucleating agents for iPP, especially at concentrations less than 5 vol%. Presence of the β‐structure crystals reduced the elastic modulus and yield strength of the nanocomposites. Micromechanical analysis showed enhanced interaction between organic and inorganic phases of the compatibilized nanocomposites. POLYM. ENG. SCI., 54:874–886, 2014. © 2013 Society of Plastics Engineers     

Interpolyelectrolyte complexes of maleic acid copolymers and chitosan for stabilization and functionalization of magnetite nano‐ and microparticles

A facile method of preparation of stabilized and functionalized nano‐ and microparticles of magnetite by successive application of oppositely charged polymers with a regular structure of macromolecular chains (chitosan and maleic acid copolymers) onto Fe₃O₄ core are developed. This approach makes it possible to create two types of magnetite interpolyelectrolyte shells, containing carboxylic or amino groups in outer layer of shell. Composition and magnetic properties of composite particles depend on nature of the copolymer of maleic acid, reaction conditions and size of obtained particles. The carboxylic groups of copolymer in outer layer of interpolyelectrolyte shell were converted into reactive anhydride groups by heating. Thermal treatment also leads to covalent crosslinking of shell and improves stability of composites both in acidic and alkaline media. Horseradish peroxidase was successfully immobilized onto covalently crosslinked and activated microparticles of Fe₃O₄ in aqueous medium without of condensing agents. The proposed reproducible and low‐cost technique does not use toxic reagents or solvents at all stages, including preparation of Fe₃O₄, formation, activation and crosslinking, of magnetite shell, modification of activated surface of composite particles. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 39663.     

Cytotoxic effect of functionalized superparamagnetic samarium doped iron oxide nanoparticles for hyperthermia application

Magnetic Fluid Hyperthermia (MFH) is an emerging and safe technique for cancer treatment. Radiotherapy and Chemotherapy are widely adopted techniques for treating cancer but cause damage to the nearby healthy tissue. This paves the way for hyperthermia treatment for cancer. Since healthy cells are more heat-tolerant than malignant cells, magnetic nanoparticles with superparamagnetic properties were used in hyperthermia treatment. Surface modified magnetite (Fe₃O₄) iron oxide nanoparticles with enhanced stability, solubility, bio-compatibility and magnetic property were employed in hyperthermia treatment. In the present study, Superparamagnetic Samarium doped magnetite (Fe₃O₄:Sm) nanoparticles were functionalized with Oleylamine (OAm) and polyvinyl alcohol (PVA) by the sol-gel process. The obtained nanoparticles were characterized by X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), Transmission Electron Microscopy (TEM), and UV–Visible diffuse reflectance spectroscopy (UV-DRS), Thermogravimetric analysis (TGA) and Vibrating Sample Magnetometer (VSM). From XRD data, the crystallite size of oleylamine coated samarium doped magnetite (OAm–Fe₃O₄:Sm) and PVA-coated samarium doped Fe₃O₄ (PVA- Fe₃O₄:Sm) were found to be 9.5 nm and 10.9 nm, respectively. TEM images of the functionalized nanoparticles were visualized as a spherical structure with reduced agglomeration. UV-DRS gives the bandgap value of OAm–Fe₃O₄:Sm and PVA- Fe₃O₄:Sm coated samarium doped magnetite to be 2.3 eV and 2 eV respectively. VSM measurement of OAm-Fe₃O₄:Sm and PVA- Fe₃O₄:Sm coated, showed superparamagnetic behaviour. The cytotoxicity study on the L929 cell line shows that both oleylamine and PVA-coated samarium doped magnetite were less toxic and biocompatible compared to the uncoated Fe₃O₄:Sm. The hyperthermia study reveals a rise in temperature within a few seconds with a high Specific Absorption Rate (SAR) value, confirming that the functionalized Samarium doped Fe₃O₄ was an effective nanomaterial for hyperthermia application.     

Electrostatic Capture Efficiency Enhancement of Polypropylene Electret Filters with Barium Titanate

This study reports on the effects of BaTiO₃—a high dielectric constant additive—addition on charging and filtration properties of meltblown polypropylene (PP) electret filters. Since electrostatic capture efficiency of electret filters is mainly dependent on electrical forces, surface potential and aerosol filtration properties were analyzed and compared. Due to quasi-permanent nature of electret property, stability of charging and filtration performance was also investigated via following an isothermal charge decay procedure. Addition of BaTiO₃ did not alter fiber morphology significantly. Particularly, the stability of electrostatic filtration performance was found to be promising with the addition of BaTiO₃. Possible microstructural changes after addition of BaTiO₃ were investigated via wide angle X-ray diffraction. Changes in crystal structure of PP upon addition of BaTiO₃ did not deteriorate electrostatic properties.

Copyright 2015 American Association for Aerosol Research     

Enhanced piezoelectric responses and crystalline arrangement of electroactive polyvinylidene fluoride/magnetite nanocomposites

The well distributed and electroactive polyvinylidene fluoride (PVDF)/magnetite nanocomposites were successfully fabricated using a mixed solvent system (THF/DMF). Dynamic mechanical properties of the fabricated PVDF/magnetite nanocomposites indicate significant enhancements in the storage modulus as compared with that of neat PVDF. By adding 2 wt % magnetite nanoparticles into the PVDF matrix, the thermal stability of nanocomposites could be enhanced about 26°C as compared with that of PVDF. The β‐phase fraction of PVDF is significantly enhanced with increasing the voltage of electric field poling. The piezoelectric responses of PVDF/magnetite films are extensively increased about five times in magnitude with applied strength of electrical field at 35 MV/m. The change of piezoelectric responses during the applied electric field may be due to the relative long arrangement of PVDF units along the direction of electric field poling and thus increases the values of L_p^* and l_c. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40941.     

Magnetite-based glass-ceramics prepared by controlled crystallization of borosilicate glasses: Effect of nucleating agents on magnetic properties and relaxation

The specific magnetic structure and magnetic relaxation phenomena in magnetite nanoentities grown in a glassy matrix by controlled crystallization of Fe-containing borosilicate and boroaluminosilicate glasses in the presence of two types of nucleating agents, Cr₂O₃ and P₂O₅, were investigated. The structure, morphology and magnetic properties are strongly influenced by the nucleating agents. Cr₂O₃ generates magnetite-based glass ceramics with magnetite configurations showing an upward relaxation of magnetization at low and high temperatures but downward at intermediate temperatures. The magnetite grown with P₂O₅ displays only downward relaxation but with different signs of the temperature derivative of the relaxation rate S in different temperature ranges. The observed effects are discussed with respect to the following factors: i) the existence of a multimodal size distribution of the magnetite (nano)particles as revealed by high resolution electron microscopy; ii) the degree of occupation of different sublattices of the magnetite structure with Fe³⁺ and Fe²⁺ ions; and iii) the interplay between the relaxation mechanisms in different temperature ranges.     

Synthesis and encapsulation of magnetite nanoparticles in PLGA: effect of amount of PLGA on characteristics of encapsulated nanoparticles

Oleic acid-coated superparamagnetic iron oxide nanoparticles (Fe₃O₄) encapsulated within poly(d,l-lactide-co-glycolide) (PLGA) particles were prepared by the w/o/w emulsion technique using poly(vinyl alcohol) as a dispersant. The concentration of PLGA in the oil phase was varied (5, 15, 30, 45, and 60?mg/ml) at constant magnetite concentration in the oil phase (5?mg/ml) to study the properties of composite Fe₃O₄–PLGA nanoparticles. Even though PLGA concentration varied widely in the oil phase, the weight percent of 7–16?nm diameter magnetite in the particles varied only from 56 to 62?% (23–28?vol.%). The obtained composite nanoparticles were essentially spherical with magnetite spatially uniformly dispersed in individual PLGA particles, as measured by transmission electron microscopy (TEM). Also, the magnetite concentration in each particle did not vary widely as determined qualitatively via microscopy. Hydrodynamic diameters of the composite nanoparticles as measured by dynamic light scattering increased by approximately 10?% with added magnetite, with a smaller relative increase in diameter measured by TEM. The zeta potential of the particles was about ?26?mV, independent of Fe₃O₄ loading. Relatively high saturation magnetizations (36–45?emu/g) were measured for these highly loaded particles, with the latter value only 7?emu/g lower than the value measured for the oleic acid-coated particles alone.     

Preparation and properties of ferromagnetic glass ceramics and glass fibers based on the composition of SiO2-B2O3-Fe2O3-SrO

The ferromagnetic glass ceramics in the system SiO₂-B₂O₃-Fe₂O₃-SrO were prepared via four different fabrication methods, i.e., fiber-drawing, melt-quenching, natural-cooling, and annealing, without performing any nucleation and crystallization heat treatments. The influences of chemical composition and fabrication method on the spontaneous crystallization of magnetite were investigated by X-ray diffraction, scanning and transmission electron microscopy. The X-ray diffraction patterns show the presence of nanometric magnetite crystals in the glass matrix, and the increasing boron oxide can promote the spontaneous crystallization of magnetite. The estimated size of crystallized magnetite varies between 12 and 50 nm. The magnetic properties of the glass ceramics derived from the four fabrication methods were analyzed using a Vibrating sample magnetometer (VSM), Agilent HP8722ES vector network analyzer and Mössbauer spectra. We find that both the saturation magnetization (M_S) and coercivity (H_jc) depend on the chemical composition and fabrication method. The calorimetric measurements were carried out using Orton Standard Dilatometers.     

Peroxide‐catalyzed swell grafting of maleic anhydride onto polypropylene

A new grafting method was developed to incorporate maleic anhydride directly onto solid‐state polypropylene powders. Maleic anhydride grafts altered the nonpolar characteristics of polypropylene so that much better mixing was achieved in blends and composites of polypropylene with many other polymers and fillers. Maleic anhydride was grafted onto polypropylene by the peroxide‐catalyzed swell grafting method, with a maximum extent of grafting of 4.60%. Fourier transform infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis, scanning electron microscopy, tensile testing, and impact testing were used to characterize the isotactic polypropylene (iPP), maleic anhydride grafted polypropylene (MAH‐g‐iPP), and (isotactic polypropylene)/(calcium carbonate) composites (iPP/CaCO₃). The crystallinity and heat of fusion of the MAH‐g‐iPP decreased as the extent of grafting increased. The mechanical properties of the CaCO₃ filled polypropylene were improved by adding MAH‐g‐iPP as a compatibilizing agent. The dispersion of the fillers in the polymer matrix and the adhesion between the CaCO₃ particles and the polymer matrix were improved by adding the compatibilizer.     

Synthesis of water dispersible magnetite nanoparticles in the presence of hydrophilic polymers

Water dispersible magnetite nanoparticles (Fe₃O₄) were synthesized by thermal decomposition of iron (III) acetylacetonate (Fe(acac)₃) in the presence of carboxylic acid-terminated poly(ethylene glycol) (mPEG acid), poly(vinyl alcohol) and NH₂-containing polyether. Crystal structure was investigated using X-ray diffractometry (XRD) and it showed that the as-synthesized particles had high crystallinity with distinct lattices. Particle size of the nanoparticles was investigated using XRD (15.32 nm), transmission electron microscopy (18.8 nm) and photo correlation spectroscopy (32 nm) techniques. Vibrating sample magnetometry indicated that magnetite nanoparticles exhibited superparamagnetic behavior at room temperature. Influence of each functional group on magnetic properties of the particles was also examined. These magnetite nanoparticles remained dispersible in aqueous dispersions with only 5% particles aggregating after 1 month of preparing.     

Flame retardation of polypropylene: Effect of silane treated antimony compounds

Flame retardation of polypropylene was accomplished by blending with antimony compounds (Sb₂O₃ and SbPO₄) in conjunction with polyvinyl chloride (PVC) or ferric oxide. The compatibility and dispersion of antimony compounds in the polymer matrix was enhanced by using silane coupling agents, viz., vinyltriethoxysilane (A-151) and γ-aminopropyltriethoxysilane (A-1100). Rheological properties of filled polypropylene were studied in the temperature range 180 to 220°C at shear rates of 29.5 to 119.5 sec^?1. An increase in the melt viscosity was found in the filled polypropylene as compared to virgin polymer. Silanation of antimony compounds also influenced the melt rheology of flame retardant polypropylene. Incorporation of 6 phr Sb₂O₃ and 19 phr PVC raised the oxygen index of polypropylene to 22.9 and this sample was found to be self extinguishing in 65 s with a burning rate of 0.06 mm/s as compared to 1.1 mm/s for unfilled polypropylene. Though silanation of antimony compounds slightly reduced the oxygen index of flame retardant polypropylene, yield strain and flexural rigidity of injection molded samples was improved over unsilanated flame retardant polymer.     

Ethylenediaminetetraacetic acid as capping ligands for highly water-dispersible iron oxide particles

Monodispersed magnetite (Fe₃O₄) particles were synthesized using a high-temperature hydrolysis reaction with the assistance of ethylenediaminetetraacetic acid (EDTA) as capping ligands. These particles were composed of small primary nanocrystals and their sizes could be tuned from about 400 to about 800 nm by simply changing the EDTA or precursor concentration. Surface-tethered EDTA made the particles highly water-dispersible. The as-prepared magnetite particles also showed superparamagnetic behavior at room temperature, and their magnetic properties were size dependent. In addition, the particles had a strong response to external magnetic field due to their high magnetization saturation values. These properties were very important for some potential biomedical applications, such as magnetic separation and magnetic-targeted substrate delivery.     

Preparation and characterization of thermoplastic vulcanizate/silica nanocomposites

This article describes the preparation, characterization, and properties of thermoplastic vulcanizate (TPV)/silica nanocomposites. The nanocomposites were prepared by the melt blending of TPV and maleic anhydride grafted polypropylene (mPP) into organically modified SiO₂ (m‐SiO₂), treated with n‐hexadecyl trimethylammonium bromide as a grafting agent for TPV during the melt mixing. The thermal stability and storage modulus of the 1 wt % m‐SiO₂ containing TPV/mPP/m‐SiO₂ nanocomposite were higher than those of pristine TPV. The most important observation was obtained from dynamic mechanical analysis, which revealed that the glass‐transition temperature of the polypropylene phase of the nanocomposites increased (in comparison with that of virgin TPV), whereas the ethylene–propylene–diene monomer phase remained almost the same. The adhesion strength between the TPV/mPP/m‐SiO₂ nanocomposites and steel also increased with increasing m‐SiO₂ content. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 2058–2063, 2005     

Magnetic properties of PAN-based carbon fibres modified with magnetite nanoparticles

The magnetic properties of PAN-based carbon fibres modified with magnetite nanoparticles are presented and analyzed. PAN fibres and PAN-based carbon fibres modified with different amounts of magnetite are characterized by the use of magnetization measurements and Mössbauer spectroscopy techniques. The investigations revealed that magnetite (Fe₃O₄) decomposed into Fe_α, Fe_γ and cementite (Fe₃C). Precise analysis of the phase’s contents for different carbon fibres has been carried out in relation to the initial magnetite compound. Analysis of the Mössbauer spectra allowed the determination of the phase contents in fibres with different initial magnetite concentrations. Partial transformation of magnetite into γ-Fe induces catalytic carbonization and formation of a highly crystalline carbon matrix at 1000 °C. The apparent crystallite size in carbon fibres containing 30% magnetite was almost seven times higher than that found in the pure carbon fibres.     

Producing PLGA fine particles containing high magnetite nanoparticles by using the electrospray technique

Loading magnetite (Fe₃O₄) nanoparticles (NPs), extensively using magnetic agents in magnetic resonance imaging (MRI) and drug delivery in a matrix of polymeric fine particles (FPs), can optimize not only the delivery of these diagnostic and therapeutic agents but also the design of multifunctional drugs. In an effort to use a new method for producing high magnetite loaded polymeric particles, oleic acid (OA) capped magnetite NPs were synthesized and loaded into biocompatible and biodegradable FPs of poly lactic-co-glycolic acid (PLGA) by using the electrospray (ES) technique; and the effect of voltage, flow rate and magnetite content on the morphology, size, size distribution, uniformity and magnetic properties of fabricated magnetic FPs (MFPs) were studied. Results of SEM images and calculations showed that solution flow rate is a major factor in ES and the particle size of magnetite loaded PLGA FPs increases considerably as the flow rate increases. Particle size did not change considerably due to an increase in voltage; however, particle uniformity first increased and then decreased due to an increase in flow rate or voltage. High magnetite content of 72% was achieved for magnetite loaded PLGA FPs and an increase in the magnetite content resulted in an increase in the saturation magnetization of magnetite loaded PLGA FPs; though, their sphericity decreased.