LDPE, EPM and their derivatives containing a moderate amount (0.08-1.8 by mol) of diethylsuccinate or succinic anhydryde groups were used as matrices in blending with different amount of organophilic montmorillonites and the resulting composite morphology and structure (by XRD, SEM, TEM microscopy, DSC analysis and selective solvent extraction) were studied with reference to the polar groups/MMT ratio. Exfoliated, intercalated and mixed morphologies were achieved. High concentrations of polar groups grafted to the polyolefin and montmorillonite loading not larger than 5% wt were favourable for obtaining high exfoliation degree. Particularly in the exfoliated MMT composite LDPE had lower crystallinity degree, while EPM showed increased glass transition temperature and reduced solubility in hot toluene. Moreover, oxygen and water vapor barrier property improvement was observed in films where MMT exhibits either exfoliated or intercalated morphologies. Strong interactions with the montmorillonite particle surface through the polar groups grafted to the polyolefin seems to be the basic effect responsible for the morphology and peculiar properties. A model based on the reduced mobility of the polymer located near the particle surface or inside the MMT gallery (confined phase) was proposed to explain the observed oxygen permeability reduction, the T(g) increase and solubility of poly(ethylene-ran-propylene)/MMT nanocomposites.

Boehmite nanoparticles covered with a polymer shell enhancing the organophilicity of the surface were prepared by physical adsorption of a polyelectrolyte atom transfer radical polymerization (ATRP) macroinitiator followed by graft-polymerization of methyl methacrylate or 2-hydroxyethyl methacrylate. The presence of polymer chains adsorbed/grafted on the Boehmite was confirmed by attenuated total reflection infrared (ATR-IR) spectroscopy and by thermo-gravimetric analysis (TGA), which showed a significant amount of polymer covering the particles. The methodology of polymerization and the kinetics suggested the possibility to modulate the amount, type and thickness of grafted polymer shell. These organic-inorganic hybrid materials were melt compounded in a Brabender mixer with isotactic polypropylene in the presence of functionalized polypropylene. The dispersion degree of Boehmite nanoparticles in the polypropylene matrix as well as their reinforcing effect were studied by morphology characterization [scanning electron microscopy (SEM) and X-ray diffraction (XRD)], whereas thermal and thermo-mechanical properties were assessed by differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA).

Atomic force microscopy (AFM) has become established as a powerful and versatile tool for investigating local mechanical properties. In addition, through the AFM tip–sample interaction, it has become possible to study the effects of perturbations and modifications to the surface of soft samples, such as polymers. The accurate knowledge of their response to continuous AFM scanning could help to design new materials having desirable mechanical properties. In this paper, we present the results obtained by applying a new methodology to investigate wear properties on two different type of polymer, poly(methyl-methacrylate) and poly(l-lactic acid). These polymers have been widely employed in biomedical applications and have recently been considered as good candidates for coronary metallic stent coatings. Copyright © 2006 John Wiley & Sons, Ltd.

Several salicylaldiminate M(II) complexes of Nickel, Copper and Cobalt have been prepared and mixed with ethylene based polymers in order to prepare new composite materials with interesting morphological and optical properties by profiting of the presence of alkyl chains and push-pull substituents connected to the ligand structure. The phase dispersion behaviour of the binary films has been studied by scanning electron microscopy (SEM) and x-ray microanalysis, whereas the optical properties of the composite samples have been evaluated by UV-vis and fluorescence spectroscopy. The results in absorption have been analysed in terms of the anisotropy induced by the mechanical orientation of the polymer matrix and by the role of the metal centre according to the different strength of the complexes transition dipole moment. The luminescence behaviour have been discussed in terms of potential developments aimed at preparing polymeric supported Schiff base ligands for metal ions sensor applications.

The study deals with the effectiveness of maleic anhydride grafted styrene-b-ethylene-co-propylene copolymer (SEPMA) as compatibilizer precursor (CP) for blends of low density polyethylene (LDPE) with polyamide-6 (PA). The CP was produced by grafting MA onto SEP in the melt. The specific interactions between the CP and the blends components have been investigated through characterizations of the binary LDPE/CP and PA/CP blends. The compatibilizing efficiency of the MA-grafted SEP, as revealed by the thermal properties and the morphology of the compatibilized blends, has been shown to be excellent. The morphology, as well as the mechanical properties of the compatibilized with SEPMA 75/25 w/w and 25/75 w/w LDPE/PA6 blends have been compared with those of the blends compatibilized with maleic anhydride functionalized HDPE sample (1-HDPE-g-MA) and with a commercial maleic anhydride grafted styrene-b-(ethylene-co-1-butene)-b-styrene copolymer (SEBSMA1). The results show that the strong compatibilizing efficiency of SEPMA is comparable with that of SEBSMA1, while 1-HDPE-g-MA exhibits a slightly lower activity, particularly for the blends, in which PA is the matrix phase.

The melt mixing of functionalized polyolefins with a surface-modified layered silicate (montmorillonite) was investigated as an approach to prepare the corresponding micro/nanocomposites. The effect of the diethyl succinate groups, derived from the grafting of diethyl maleate (DEM) onto the polyolefins, on compatibility with an inorganic filler and the dispersion in a hydrophobic matrix was extensively investigated. In order to avoid possible interference by polymer multiphase morphology, the amorphous poly(propylene-ran-ethylene) (EPM) (70/30, wt/wt), functionalized with DEM (EPM-graft-DEM), was used in melt mixing with alkyl-ammonium-salt-modified montmorillonite at different weight ratios by using a Brabender mixer. Materials with a nanoscale dispersion of the inorganic phase, as revealed by X-ray diffraction (XRD) and transmission electron microscopy (TEM) analyses, were obtained. Specific interactions, involving the carbonyl groups of the polyolefin functional groups and the polar sites on the filler surface, appeared to assist intercalation and/or exfoliation of the layered system. Similar results were obtained by starting with an unfunctionalized EPM and by performing the grafting reaction with DEM during melt mixing according to a one-step simplified procedure. (c) 2005 Society of Chemical Industry.

The phase morphology of blends of low density polyethylene (PE) with low molecular weight copolyamide (CPA) was investigated in films having 50-100 mu m thickness. Films were prepared by compression Moulding between two surfaces with different polarity, namely teflon and aluminium sheets, in a parallel plate heating press. The film Surface characterization and surface energy deduction were performed by FT-IR/ATR spectroscopy and contact angle measurements, respectively. Moreover, the morphology and phase distribution were investigated by scanning electron microscopy both on the surfaces and oil the cryogenic section of the films.The copolyamide resulted to be the dispersed phase in all compositions (90/10, 95/5, 97.5/2.5 and 99/1 PE/CPA) and the shape, dimension and distribution of the domains depending on temperature, Pressure, time and nature of the surfaces used during the compression stage.The experimental evidences were discussed with respect to the different Surface energies of the type of moulding material during the film, preparation and related compatibility of the components. (c) 2005 Elsevier Ltd. All rights reserved.

Four different types of montmorillonites have been dispersed by sonication at 50 degrees C into a propoxylated aromatic epoxy diacrylate oligomer to achieve interlayered or exfoliated nanocomposites. A thermally-induced cross-linking reaction, forming a polyurethane network in the presence of 7 wt.-% of a montmorillonite, has been promoted by addition of an allophanate modified polyisocyanurate based on hexamethylene diisocyanate. The kinetic behavior of the network formation has been studied at 25, 40 and 60 degrees C by following the disappearance of the isocyanate vibrational band found at 2 270 cm(-1). A tight crosslinked polyurethane acrylate network has been achieved by a subsequent dual UV curing promoted by a photoinitiator mixture (0.6 wt,-%) added to the reactive mixture because of further reactions occur to the acrylate double bonds. The photopolymerization kinetic has been investigated on the different thermally treated polyurethane nanocomposite networks by Real Time FTIR spectroscopy monitoring the changes of the IR band at 810 cm(-1) assigned to the acrylate double bond vibrations. The influence of the different montmorillonite clays on the final nanocomposite morphology has been investigated by using XRD and SEM. Finally, the use of these mixtures as internal layer between two modified surface PET films has been also studied for the laminate production. The based-PET laminate films have been characterized by determining the bending resistance and optical properties as a function of different nanofillers.

In the present paper, adhesion force between a phospholipid (Lecithin of Soya) and a series of biodegradable polyurethanes (PUs) was investigated by means of an atomic force microscope (AFM). Force–distance curves were recorded in aqueous solution making use of a phospholipid-coated probe tip. In addition, micro/nanoscale mechanical characterization of polymer samples was addressed to understand how surface properties could favor cell growth. The technique could become a useful method to select the best candidate materials for 3D scaffolds realisation for tissue engineering.

Atomic Force Microscopy (AFM) has become established as a powerful and a versatile tool for investigating local mechanical properties. In addition, it has been made possible to take advantage of the AFM tip-sample interaction, to perturb, and I turn, to modify the surface of soft samples, such as polymers. The accurate knowledge of their response to the continuous AFM scanning could help to design new materials having desirable mechanical properties. In this paper, we present the results obtained applying a new methodology to investigate wear properties on two different type of polymers, such as poly(methyl methacrylate (PMMA) and poly(L-lactic acid) (PLLA). These polymers have been widely employed in biomedical applications and have recently been considered as good candidates for coronary metallic stent coatings.

Attempts have been performed to obtain spectroscopic evidence of intermolecular interactions between fluorinated polymers to be used as protective materials and various stones. In this paper we report an investigation by means of FTIR spectroscopy on poly(vinyl fluoride)(PVF) which contains acid hydrogens that can give rise to intermolecular interactions with calcium carbonate. Spectral changes have been found in the CH and CF stretching regions at 3000–2840 and 1200–950 cm −1 , respectively. These last are attributed to intermolecular interactions of the polymer with CO 3 2− and with conformational changes of the macromolecular chain. Scanning electron microscopy investigations were also performed on marble slabs coated with a PVF film in order to gain information about the morphology of the polymer film. Copyright © 2004 Society of Chemical Industry

The porosity evolution in heavy oil fly ashes subjected to activation with CO2, has been examined. The work examined four different heavy oil fly ashes that, after preliminary acid leaching, have been pyrolyzed at 900 degreesC and then activated with CO2 at the same temperature for different times.A different evolution of porosity was observed according to the different reactivity of the samples during activation. The activated samples have been characterised as regards the surface area and the pore volume. The scanning electron microscope-energy dispersive spectrometer microanalysis has been used to interpret the experimental results. (C) 2003 Elsevier Science Ltd. All rights reserved.

The use of heavy oil fly ash with high ash content (45 wt.%) as a precursor for the preparation of activated carbons has been investigated. The raw fly ash and the fly ash with lower ash content, obtained by a HCl/HF washing treatment, have been pyrolyzed at 900 degrees C and then activated with CO(2) in the temperature range of 800-900 degrees C for different times. The activated carbons have been characterised as regards the surface area and the pore volume. The evolution of the porosity has been related to the burn-off degree.

Composites between alumina and the bioresorbable poly(ε-caprolactone)-block-poly(oxyethylene)-block-poly(ε-caprolactone) copolymer were obtained by reacting ε-caprolactone with preformed poly(ethylene glycol), in the presence of ceramic alumina powder, at 185°C under vacuum. The mechanical properties, tested by compression and flexural strengths and Young's modulus, show that the copolymer interacts poorly with the alumina grains. Both scanning electron and atomic force microscopy show a scarce wettability between alumina and copolymer, as well as the aggregation of alumina micro-particles into clusters of big size. Both mechanical and morphological tests seem to indicate a stronger interaction between the alumina micro-particles than between the alumina surface and the reaction mixture during the polymerization, as well as a “compacting effect” by alumina on the forming copolymer. The FT-IR spectra of the composites show both copolymer and alumina absorption bands. The FT-IR analysis on the fractions of an extraction with CHCl3 indicates the presence of traces of poly(ε-caprolactone), stably linked to alumina. The polymerization of ε-caprolactone with alumina alone in the same conditions gives poly(ε-caprolactone), mainly free and in minor part linked to the alumina surface. Two polymerization mechanisms, simultaneously occurring, are proposed. The most relevant result of this work is the lack of chemical inertness of alumina towards ε-caprolactone, which leads to reconsider also the use of alumina as a biochemically inert material.

BACKGROUND AND PURPOSE:In the 1990s, the introduction of the Guglielmi detachable coil (GDC) system in clinical practice was followed by extensive clinical use of this endovascular device in the treatment of brain aneurysms. This technology is based on electrothrombosis and electrolytic detachment of platinum coils. Despite the extensive use of this treatment technique, the role of electrothrombosis has not been fully investigated and clarified. An in vitro electron microscopic study of human blood was performed to elucidate the role that electrothrombosis might play in triggering the biologic response of thrombosis of the aneurysmal sac.METHODS:Human blood from five patients was used to fill plastic containers in which GDCs had been deposited. These five patients had subarachnoid hemorrhage and were similar in age and clinical presentation. Electron microscopic studies were performed on GDCs that had been electrically charged and on GDCs that had not.RESULTS:All electron microscopic studies revealed that the electrically charged GDCs were covered by blood elements and fibrin adherent to the surface of the coil. Noncharged GDCs did not have deposits or adhesions of these blood constituents.CONCLUSION:These findings demonstrated that passage of electric current through the GDC induces attraction of blood constituents. This attraction may trigger a thrombotic reaction on the surface of the coil. The greater the time of current application, the more pronounced the cellular reaction and the deposition of fibrin and blood cells on the GDC.

"Synthetic blends" of a flexible polymer forming the matrix and a liquid-crystalline polymer (LCP) forming the dispersed phase have been prepared by transesterification of PET with a mixture of sebacic acid (S), 4,4'-diacetoxybiphenyl (B) and 4-acetoxybenzoic acid (H) in the mole ratio 1:1:2. A change of the synthesis condi tions causes marked variations of the chemical composition and the morphology of the phases. The SEM investigation of the inner morphology of the LCP droplets of blends consisting of two phases with fairly different aromatic content has shown that the LCP macromolecules are aligned tangentially at the matrix surface boundary, and that the nematic director configuration is toroidal. When the two phases have closer chemical composition, and are therefore supposed to possess improved mutual compatibility, a perpendicular anchoring of the LCP fibrils to the matrix cavity surface, and an axial configuration of the nematic director, are observed. The expected effect of the nematic configuration of the LCP droplets on their ability to deform into fibrils under appropriate flow conditions is preliminarily discussed.

Histologic findings after Guglielmi detachable coils endovascular embolisation have been studied in experimental aneurysms. Few reports describe histopathologic reactions to platinum coils in humans. In this report we describe gross, light microscopic pathology and scanning electron microscopy study of a ruptured basilar tip artery aneurysm in a patient who died 16 hours following coiling.