References of "Calberg, Cédric"
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See detailExfoliated polylactide/clay nanocomposites by in-situ coordination-insertion polymerization
Paul, Marie-Amélie; Alexandre, Michaël ULg; Degée, Philippe et al

in Macromolecular Rapid Communications (2003), 24(9), 561-566

Poly(L-lactide)/layered aluminosilicate nanocomposites were synthesized in bulk by ring-opening polymerization in the presence of two organo-modified montmorillonites. When the organo-modifier consisted ... [more ▼]

Poly(L-lactide)/layered aluminosilicate nanocomposites were synthesized in bulk by ring-opening polymerization in the presence of two organo-modified montmorillonites. When the organo-modifier consisted of an ammonium cation bearing primary hydroxyl groups, polymerization was initiated by the alcohol functions after adequate activation. The growing polymer chains were directly "grafted" onto the clay surface through the hydroxyl-functionalized ammonium cations yielding exfoliated nano-composites with enhanced thermal stability. [less ▲]

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See detailSupercritical carbon dioxidce technology: a new method for the preparation of green materials
Stassin, Fabrice; Calberg, Cédric ULg; Pagnoulle, Christophe et al

Poster (2003, May 16)

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See detailPolymer functionalized multi-walled carbon nanotubes
Petrov, Petar; Pagnoulle, Christophe; Stassin, Fabrice et al

Poster (2003, May 16)

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See detailPolymer/layered silicate nanocomposites by combined intercalative polymerization and melt intercalation: a masterbatch process
Lepoittevin, Bénédicte; Pantoustier, Nadège; Devalckenaere, Myriam et al

in Polymer (2003), 44(7), 2033-2040

Poly(ε-caprolactone) (PCL) and poly(vinyl chloride) (PVC) layered silicate nanocomposites were prepared by combination of intercalative polymerization and melt intercalation. In a first step, high clay ... [more ▼]

Poly(ε-caprolactone) (PCL) and poly(vinyl chloride) (PVC) layered silicate nanocomposites were prepared by combination of intercalative polymerization and melt intercalation. In a first step, high clay content PCL nanocomposites were prepared by in situ polymerization of -caprolactone intercalated between selected organo-modified silicate layers. The polymerization was catalyzed with dibutyltin dimethoxide in the presence of montmorillonites, the surface of which were previously exchanged with (functionalized) long alkyl chains ammonium cations. Then, these highly filled PCL nanocomposites were added as masterbatches in commercial PCL and PVC by melt blending. The intercalation of PCL chains within the silicate layers by in situ polymerization proved to be very efficient, leading to the formation of intercalated and/or exfoliated structures depending on the organo-clay. These masterbatches were readily dispersed into the molten PCL and PVC matrices yielding intercalated/exfoliated layered silicate nanocomposites which could not be obtained by melt blending the matrix directly with the same organo-modified clays. The formation of nanocomposites was assessed both by X-ray diffraction and transmission electronic microscopy. Interestingly, this so-called 'masterbatch' two-step process allowed for preparing PCL nanocomposites even with non-modified natural clay, i.e. sodium montmorillonite, which showed a material stiffness much higher than the corresponding microcomposites recovered by direct melt intercalation. The thermal stability of PCL nanocomposites as a function of clay content was investigated by thermogravimetry (TGA). [less ▲]

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See detailPoly(epsilon-caprolactone)/clay nanocomposites by in-situ intercalative polymerization catalyzed by dibutyltin dimethoxide
Lepoittevin, Bénédicte; Pantoustier, Nadège; Devalckenaere, Myriam et al

in Macromolecules (2002), 35(22), 8385-8390

Poly(epsilon-caprolactone)/clay nanocomposites were prepared by in-situ ring-opening polymerization of epsilon-caprolactone by using dibutyltin dimethoxide as an initiator/catalyst. A nonmodified Na ... [more ▼]

Poly(epsilon-caprolactone)/clay nanocomposites were prepared by in-situ ring-opening polymerization of epsilon-caprolactone by using dibutyltin dimethoxide as an initiator/catalyst. A nonmodified Na+-montmorillonite and two montmorillonites surface-modified by dimethyl 2-ethylhexyl (hydrogenated tallow alkyl) and methyl bis(2-hydroxyethyl) (hydrogenated tallow alkyl) ammonium cations, respectively, were used. The evolution of molecular weights was followed in relation to silicate surface modification and clay concentration. The alcohol-bearing organo-modified clay was a co-initiator for the polymerization reaction and thus controlled the molecular weight of the PCL chains. Furthermore, the number-average molecular weight of the growing PCL chains linearly increased with the monomer conversion. Nanocomposites were analyzed by small-angle X-ray diffraction, transmission electron microscopy, and thermogravimetry. The clay dispersion depended on the structure of the alkylammonium used to make the clay more hydrophobic. Exfoliated nanocomposites were formed when hydroxyl-containing alkylammonium. was used; otherwise, intercalated structures were reported. Thermogravimetric analyses showed a higher degradation temperature for the exfoliated structures than for the intercalated ones, both of them exceeding the degradation temperature of unfilled poly(epsilon-caprolactone). [less ▲]

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See detailBiodegradable polyester layered silicate nanocomposites based on poly(epsilon-caprolactone)
Pantoustier, Nadège; Lepoittevin, Bénédicte; Alexandre, Michaël ULg et al

in Polymer Engineering & Science (2002), 42(9), 1928-1937

Nanocomposites based on biodegradable poly(epsilon-caprolactone) (PCL) and layered silicates (montmorillonite, MMT) were prepared either by melt intercalation with PCL or by in situ ring-opening ... [more ▼]

Nanocomposites based on biodegradable poly(epsilon-caprolactone) (PCL) and layered silicates (montmorillonite, MMT) were prepared either by melt intercalation with PCL or by in situ ring-opening polymerization of epsilon-caprolactone as promoted by the so-called coordination-insertion mechanism. Both non-modified clays (Na+-MMT) and silicates modified by various alkylammonium cations were studied. Mechanical and thermal properties were examined by tensile testing and thermogravimetric analysis. Even at a filler content as low as 3 wt% of inorganic layered silicate, the PCL-layered silicate nanocomposites exhibited improved mechanical properties (higher Young's modulus) and increased thermal stability as well as enhanced flame retardant characteristics as a result of a charring effect. It was shown that the formation of PCL-based nanocomposites depended not only on the nature of the ammonium cation and related functionality but also on the selected synthetic route, melt intercalation vs. in situ intercalative polymerization. Interestingly enough, when the intercalative polymerization of epsilon-caprolactone was carried out in the presence of MMT organo-modified with ammonium cations bearing hydroxyl functions, nanocomposites with much improved mechanical properties were recovered. Those hybrid polyester layered silicate nanocomposites. were characterized by a covalent bonding between the polyester chains and the clay organo-surface as a result of the polymerization mechanism, which was actually initiated from the surface hydroxyl functions adequately activated by selected tin (II) or tin (IV) catalysts. [less ▲]

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See detailLayered silicate/polyester nanohybrids by controlled ring-opening polymerization
Lepoittevin, Bénédicte; Pantoustier, Nadège; Alexandre, Michaël ULg et al

in Macromolecular Symposia (2002), 183

In this study, layered silicate/aliphatic polyester nanohybrids were synthesized by ring-opening polymerization of c-caprolactone as promoted by the so-called coordination-insertion mechanism. These ... [more ▼]

In this study, layered silicate/aliphatic polyester nanohybrids were synthesized by ring-opening polymerization of c-caprolactone as promoted by the so-called coordination-insertion mechanism. These nanocomposites were formed in presence of montmorillortite surface-modified by ammonium cations bearing hydroxyl group(s), such as bis(2-hydroxyethyl)methyl (hydrogenated tallow alkyl) ammonium. The lactone polymerization could in initiated by all the hydroxyl functions available at the clay surface, after activation into either tin(II) or AI(III) alkoxide active species. Hybrid nanocomposites were accordingly generated through the covalent grafting of every polyester chain onto the filler surface. Surface-grafted polycaprolactone (PCL) chains were untied and isolated by ionic exchange reaction with LiCl in THF solution and molar masses were measured by size exclusion chromatography. The PCL molar masses could be controlled and readily tuned by the content of hydroxyl groups available at the clay surface. Interestingly, initiation reaction by aluminum trialkoxide active species yielded grafted PCL chains characterized by very narrow molecular weight distribution (M-w/M(n)similar to1.2). These polyester-grafted layered silicate nanohybrids displayed complete exfoliation of silicate sheets as shown by X-ray diffraction (XRD) and transmission electron microscopy (TEM). [less ▲]

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See detailPoly(epsilon-caprolactone)/clay nanocomposites prepared by melt intercalation: mechanical, thermal and rheological properties
Lepoittevin, Bénédicte; Devalckenaere, Myriam; Pantoustier, Nadège et al

in Polymer (2002), 43(14), 4017-4023

(Nano)composites of poly(epsilon-caprolactone) (PCL) were prepared by melt blending the polymer with natural Na+ montmorillonite and montmorillonite modified by hydrogenated tallowalkyl (HTA)-based ... [more ▼]

(Nano)composites of poly(epsilon-caprolactone) (PCL) were prepared by melt blending the polymer with natural Na+ montmorillonite and montmorillonite modified by hydrogenated tallowalkyl (HTA)-based quaternary ammonium cations, such as dimethyl 2-ethylhexyl HTA ammonium and methyl bis(2-hydroxyethyl) HTA ammonium. Microcomposites or nanocomposites were prepared depending on whether neat or modified montmorillonites was used, as assessed by X-ray diffraction and transmission electron microscopy. Mechanical and thermal properties were studied as a function of the filter content by tensile testing, Izod impact testing, thermogravimetric analysis and differential scanning calorimetry. The rheological behaviour at 80 degreesC was also analysed in relation to the structure and content of the layered silicate. Effect of exfoliated silicates on the mechanical properties, thermal stability and flame resistance of PCL was considered. Stiffness and thermal stability improved with the filler loading until a content of 5 wt%. Further loading resulted in the levelling off and possibly in a decrease of these properties. A marked charring effect was observed upon exposure to a flame. [less ▲]

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See detailPolyester layered silicate nanohybrids by controlled grafting polymerization
Lepoittevin, Bénédicte; Pantoustier, Nadège; Alexandre, Michaël ULg et al

in Journal of Materials Chemistry (2002), 12(12), 3528-3535

Poly( epsilon-caprolactone) (PCL) layered silicate nanohybrids were synthesized by ring opening polymerization of epsilon-caprolactone according to a well-controlled coordination-insertion mechanism ... [more ▼]

Poly( epsilon-caprolactone) (PCL) layered silicate nanohybrids were synthesized by ring opening polymerization of epsilon-caprolactone according to a well-controlled coordination-insertion mechanism. Montmorillonites were surface-modified by non functional (trimethylhexadecylammonium) and hydroxy functional alkylammonium cations, i.e., (2-hydroxyethyl) dimethylhexadecylammonium. The hydroxy functions available at the clay surface were activated into tin( II or IV) or Al(III) alkoxide initiators for lactone polymerization, thus yielding surface-grafted PCL chains. The surface-grafted PCL chains were recovered by an ionic exchange reaction with lithium chloride and they were analyzed by size exclusion chromatography. The PCL molar mass was measured as a function of the hydroxy content of the clay that was modulated by exchanging the Na cations with mixtures of non-functional and hydroxy functional ammonium cations of different compositions. Nanohybrids were also characterized by small-angle X-ray diffraction, transmission electron microscopy and thermogravimetry. The PCL molar mass and the nanocomposite morphology (i.e., exfoliation and/or intercalation) were readily tuned by the content of the hydroxy groups available at the clay surface. Surface-grafted aluminium trialkoxide species proved highly efficient in initiating polymerization that leads to PCL chains of controlled molar mass and narrow molecular weight distribution with polydispersity indices as low as 1.2. [less ▲]

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See detailFull-electrochemical preparation of conducting/insulating binary polymer films
Jérôme, Christine ULg; Geskin, V.; Lazzaroni, Roberto et al

in Chemistry of Materials (2001), 13(5), 1656-1664

Binary polymer films consisting of an insulating polymer and a conducting polymer have been successfully prepared by sequential electropolymerization of the parent monomers. The insulating polymer ... [more ▼]

Binary polymer films consisting of an insulating polymer and a conducting polymer have been successfully prepared by sequential electropolymerization of the parent monomers. The insulating polymer (polyacrylonitrile or polyethylacrylate) is formed under cathodic polarization in a potential range where the growing chains are chemically grafted onto the nickel or carbon electrode. The conducting polymer (polybithiophene or polypyrrole) is formed by electrooxidation of the parent monomer. The electrochemical reactions and the electrochemical properties of the films have been analyzed by cyclic voltammetry and chronoamperometry. The influence of the main experimental parameters on the composition and morphology of the films has been investigated by X-ray photoelectron spectroscopy and atomic force microscopy. This approach strongly improves the adhesion of the conducting polymer as a result of its combination with the grafted polyacrylonitrile. This combination of insulating and conducting polymers is a way to tune the electroactivity of the conjugated chains. [less ▲]

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See detailPoly(e-caprolactone) layered silicate nanocomposites: effect of clay surface modifiers on the melt intercalation process
Pantoustier, Nadège; Alexandre, Michaël ULg; Degée, Philippe et al

in e-Polymers (2001), (9), 1-9

Nanocomposites based on biodegradable poly(e-caprolactone) (PCL) and layered silicates (montmorillonite) modified by various alkylammonium cations were prepared by melt intercalation. Depending on whether ... [more ▼]

Nanocomposites based on biodegradable poly(e-caprolactone) (PCL) and layered silicates (montmorillonite) modified by various alkylammonium cations were prepared by melt intercalation. Depending on whether the ammonium cations contain non-functional alkyl chains or chains terminated by carboxylic acid or hydroxyl functions, microcomposites or nanocomposites were recovered as shown by X-ray diffraction and transmission electron microscopy. Mechanical and thermal properties were examined by tensile testing and thermogravimetric analysis. The layered silicate PCL nanocomposites exhibited some improvement of the mechanical properties (higher Young's modulus) and increased thermal stability as well as enhanced flame retardant characteristics as result of a charring effect. This communication aims at reporting that the formation of PCL-based nanocomposites strictly depends on the nature of the ammonium cation and its functionality, but also on the selected synthetic route, i.e. melt intercalation vs. in situ intercalative polymerization. Typically, protonated w-aminododecanoic acid exchanged montmorillonite allowed to intercalate e-caprolactone monomer and yielded nanocomposites upon in situ polymerization, whereas they exclusively formed microcomposites when blended with preformed PCL chains. In other words, it is shown that the formation of polymer layered silicate nanocomposites is not straightforward and cannot be predicted since it strongly depends on parameters such as ammonium cation type and functionality together with the production procedure, i.e., melt intercalation, solvent evaporation or in situ polymerization [less ▲]

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See detailThe use of conducting polymers as cathodes for the electrochemical deposition of magnetic transition metal/rare alloys
Martinot, Lucien; Leroy, Delphine ULg; Zhan, H. et al

in Journal of Materials Chemistry (2000), 10(3), 729-735

We report the electrodeposition of Cu and Ni in aqueous solutions together with the deposition of lanthanides (Gd, Sm, Dy, Tb) and amorphous magnetic alloys of lanthanides with transition metals (Fe, Co ... [more ▼]

We report the electrodeposition of Cu and Ni in aqueous solutions together with the deposition of lanthanides (Gd, Sm, Dy, Tb) and amorphous magnetic alloys of lanthanides with transition metals (Fe, Co) onto various polymer cathodes in formamide solutions. We used conducting polymers (polypyrrole, PPy; polyethylenedioxythiophene, PEDOT) sprayed on different substrates and in addition composite materials based on carbon black (CB) mixed either with polyethylene (PE) or with polycarbonate (PC). In the latter case, the conducting material is easily shaped out in various forms. When deposited on some of these substrates, the alloys appear as an interesting material for magneto-optic recording. The electrochemical process was used for the preparation of Gd/Co and Dy/Fe alloys for which the measured coercitive fields ranged from 250–300 Oe (Dy/Fe) to about 350 Oe (Gd/Fe). We demonstrated also the feasibility of an additional electrografting of a transparent protective layer of polyacrylonitrile (PAN) in order to avoid the corrosion of the alloys by the atmosphere. [less ▲]

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See detailElectrical and dielectric properties of carbon black filled co-continuous two-phase polymer blends
Calberg, Cédric ULg; Blacher, Silvia ULg; Gubbels, F. et al

in Journal of Physics D - Applied Physics (1999), 32(13), 1517-1525

The electrical and dielectric properties of co-continuous polystyrene (PS)/ρoly(methylmethacrylate)(PMMA) blends loaded with carbon black (CB) of a special grade (BP 1000) have been studied. They strongly ... [more ▼]

The electrical and dielectric properties of co-continuous polystyrene (PS)/ρoly(methylmethacrylate)(PMMA) blends loaded with carbon black (CB) of a special grade (BP 1000) have been studied. They strongly depend on the selective localization of the CB particles at the blend interface quite consistently with the double percolation concept. The interfacial localization of CB contributes to the stabilization of the phase morphology against thermal post treatment. Nevertheless, the sample annealing has a very favourable effect on the percolation threshold that decreases The composition range in which phases are co-continuous is also increased by the addition of the filler. Dispersion of the conductance and the dielectric constant has been measured in the wide frequency range 10-4-108 Hz for blends containing 0-5 wt% CB. On the basis of these results, the mechanism of electrical transport (trapping, hopping, tunnelling, percolation) has been discussed in relation to the CB loading and the optimum loading has been identified for the electrical and dielectric properties to be stable and reproducible [less ▲]

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See detailDynamic mechanical thermal and infrared analyses of polyacrylonitrile "electrografted" onto a metal
Calberg, Cédric ULg; Mertens, Marc; Baute, Noëlle et al

in Journal of Polymer Science. Part B, Polymer Physics (1998), 36(4), 543-553

Polyacrylonitrile (PAN) films have been grafted onto copper electrodes by cathodic polarization and analyzed by infrared spectroscopy and dynamic mechanical thermal analysis (DMTA). The dynamic mechanical ... [more ▼]

Polyacrylonitrile (PAN) films have been grafted onto copper electrodes by cathodic polarization and analyzed by infrared spectroscopy and dynamic mechanical thermal analysis (DMTA). The dynamic mechanical response shows two or three transitions depending on the film thickness and the potential deposition. The viscoelastic properties of ungrafted PAN films, e.g., solvent cast films of commercially available PAN, are deeply different from those of electrografted films. The experimental data support that ungrafted chains are paracrystalline in contrast to the grafted ones which are essentially amorphous. Moreover, the irreversible transformation of the grafted PAN chains observed beyond 225°C is confirmed by Fourier transform infrared (FTIR) analysis and ascribed to an intramolecular cyclization of PAN into polyimine. This reaction occurs rapidly and at a comparatively low temperature with respect to ungrafted PAN, which suggests that the grafted chain configuration might be predominantly isotactic. The isotacticity and the amorphous structure appear to decrease as the thickness of the PAN film is increased. Literature data and the herein reported observations would suggest a dependence of the amorphous structure of PAN on the chain isotacticity. [less ▲]

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See detailSolvent effect on the electrografting of acrylonitrile on nickel
Mertens, Marc; Calberg, Cédric ULg; Baute, Noëlle et al

in Journal of Electroanalytical Chemistry (1998), 441(1-2), 237-244

The effect of solvent on the reductive electrografting of acrylonitrile (AN) onto nickel cathodes has been studied in dimethylformamide (DMF), a solvent for polyacrylonitrile (PAN), and in non-solvents ... [more ▼]

The effect of solvent on the reductive electrografting of acrylonitrile (AN) onto nickel cathodes has been studied in dimethylformamide (DMF), a solvent for polyacrylonitrile (PAN), and in non-solvents that include acetonitrile (ACN), propylene carbonate (PC) and pyridine (PY). Electrografting responsible for the cathode inhibition has been observed for the first time in PC and PY. Not only the polymer-solvent interactions but also the intrinsic polarity of the solvent have an effect on the intensity of the inhibition peak which is the signature of the electrografting reaction. Concentration of the monomer in the electrode double layer appears to decrease as the solvent polarity is increased, consistently with a more efficient displacement of the monomer by a more polar compound. That such a competition occurs is also supported by the effect of the nature and concentration of the conducting salt. The best quality films are formed in DMF, which is a solvent for PAN. Quartz microbalance experiments have emphasized the crucial importance of the potential range used for the AN electroreduction, particularly in a solvent of the polymer. [less ▲]

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See detailElectrochemistry of N-vinyl-2-pyrrolidone and a non polymerizable analogue
Calberg, Cédric ULg; Kroonen, D.; Mertens, Marc et al

in Polymer (1998), 39(1), 23-29

According to previous studies, the electropolymerization of N-vinyl-2-pyrrolidone fits a cationic mechanism with grafting of the polymer onto the platinum anode. However, this article shows that the ... [more ▼]

According to previous studies, the electropolymerization of N-vinyl-2-pyrrolidone fits a cationic mechanism with grafting of the polymer onto the platinum anode. However, this article shows that the pyrrolidone substituent of N-VP is also involved in the anodic reaction in addition to the polymerizable vinyl double bond. This additional reaction in the potential range of interest was confirmed by the electrochemical oxidation of a non polymerizable analogue of N-VP, i.e. N-methylpyrrolidone. Therefore, at least two mechanisms can contribute to the electrodeposition of a polymer film in a solvent of poly N-VP: electrografting and polymer branching and/or crosslinking by species stemming from the electrooxidation of the pyrrolidone rings. [less ▲]

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See detailBonding electropolymerization: a new electron-transfer strategy for the tailoring of performant polymer-based composites
Baute, Noëlle; Calberg, Cédric ULg; Dubois, Philippe ULg et al

in Macromolecular Symposia (1998), 134

Careful control of experimental conditions in the cathodic electropolymerization of acrylonitrile allows the grafting of thin polymer films, on conducting surfaces offering electrons easily mobilized at a ... [more ▼]

Careful control of experimental conditions in the cathodic electropolymerization of acrylonitrile allows the grafting of thin polymer films, on conducting surfaces offering electrons easily mobilized at a relatively low potential. Matching relative polarity and donicity of solvent and monomer expands the applicability of this methodology to the whole class of (meth)acrylic monomers, paving the way to many new and useful multiphase materials. [less ▲]

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See detailCharacterization of polyacrylonitrile films grafted onto nickel by ellipsometry, atomic force microscopy and X-ray reflectivity
Calberg, Cédric ULg; Mertens, Marc; Jérôme, Robert ULg et al

in Thin Solid Films (1997), 310(1-2), 148-155

The thickness and roughness of polyacrylonitrile films electrografted on a nickel surface have been measured by ellipsometry, atomic force microscopy and X-ray reflectivity. From combined ellipsometry and ... [more ▼]

The thickness and roughness of polyacrylonitrile films electrografted on a nickel surface have been measured by ellipsometry, atomic force microscopy and X-ray reflectivity. From combined ellipsometry and X-ray reflectivity measurements, accurate values for the refractive indices of polyacrylonitrile and nickel have been derived at a 6328-Åwavelength. Dependence of the film thickness on the monomer concentration has been quantified for the first time. Furthermore, the thickness of the polyacrylonitrile (PAN) film is related to the nature of the solvent, depending on whether it is a good solvent for PAN (dimethylformamide; DMF) or not (acetonitrile; ACN). [less ▲]

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See detailCarbon black-filled polymer blends : a scanning probe microscopy characterization
Leclère, Philippe; Lazzaroni, Roberto; Gubbels, Frédéric et al

in Materials Research Society Symposium Proceedings (1997), 457

Conducting polymer composites, that consist of a conducting filler randomly distributed throughout an insulating polymer or polymer blend, attract interest in several application fields such as sensors or ... [more ▼]

Conducting polymer composites, that consist of a conducting filler randomly distributed throughout an insulating polymer or polymer blend, attract interest in several application fields such as sensors or electromagnetic radiation shielding. The macroscopic electrical resistivity of the filled polyblend strongly depends on the localization of the filler. Here, we investigate the morphology of Carbon Black (CB)-filled polymer blends in order to determine the parameters governing the selective localization of CB in one phase of the blend components or at the interface between the components. The dispersion of the CB particles in the polymer blend is observed by means of Lateral Force Microscopy (LFM) as a function of the blend composition and the load in CB. The selective localization of CB at the interface enables the reduction of the percolation threshold down to 0.5 wt%; as a result, the mechanical properties of the polymer blend can be fully retained. Different techniques can be used to locate the CB at the interface; we compare their efficiency experimentally. [less ▲]

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