References of "Detrembleur, Christophe"
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See detailHigh-quality thin graphene films from fast electrochemical exfoliation
Aqil, Abdelhafid ULg; Ouhib, Farid ULg; Detrembleur, Christophe ULg et al

Poster (2013, November)

Many methods have been developed in the last few decades to obtain high-quality graphene thin sheets. They are based on very different physicochemical processes. Here we demonstrate a novel one step and ... [more ▼]

Many methods have been developed in the last few decades to obtain high-quality graphene thin sheets. They are based on very different physicochemical processes. Here we demonstrate a novel one step and simple electrografting acrylate monomer method to exfoliate highly oriented pyrolytic graphite (HOPG) into thin nanoplatelets and even down to the single graphene sheet level. Among the high research activity in the area of surface modification, electrografting is a very powerful method which has received comparatively little attention. This is surprising because this technique has many attractive features for modification of conducting or semi-conducting surfaces. The main interest of the electrografting process is to solve the recurrent problem of the organic/substrates interface weakness. The electrografting warranties a robust polymer/substrates interface and offers the possibility to tailor the functionality of the grafted polymer film opening the door to a wide range of demanding technological applications. The graphene sheets obtained through electrografting process give a stable suspension in dimethyl formamide (DMF), and they can self-precipitate on the surface of substrates after adding water as an antisolvent due to their strong surface hydrophobicity. Interestingly, the continuous films obtained exhibit ultratransparency (∼98% transmittance), and the lateral size of the exfoliated graphene sheets observed by AFM ~1nm. Raman and TEM characterizations corroborate that the graphene sheets exfoliated by our electrochemical method preserve the intrinsic structure of grapheme and give preferentially monolayered graphene sheets. The electrochemical behaviour of the acrylate monomer grafted graphene sheets was evaluated in lithium-half cells with no addition of conductive additive or binder. The PAN grafted graphene dispersed in DMF was coated on Cu foil and dried in a vacuum oven at 55°C for 12h. After 200 cycles, the reversible capacity was still kept at 300mAh/g at the current density of 50mA/g. These results indicate that the prepared high quality graphene sheets possess good electrochemical performances for lithium storage. This work provides an efficient approach to obtain high-quality, cost-effective, and scalable production of “graphene ink”, which may pave a way toward future applications in lithium- ion batteries. [less ▲]

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See detailCross-linkable polythiophene diblock copolymers: toward high thermally stable organic solar cells
Ouhib, Farid ULg; Tomassetti, Mirco ULg; Manca, Jean et al

Conference (2013, November)

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See detailNovel and simple electrografting monomer method to exfoliate HOPG for lithium-ion batteries
Aqil, Abdelhafid ULg; Ouhib, Farid ULg; Jérôme, Christine ULg et al

Conference (2013, October 28)

Many methods have been developed in the last few decades to obtain high-quality graphene thin sheets. They are based on very different physicochemical processes. Here we demonstrate a novel one step and ... [more ▼]

Many methods have been developed in the last few decades to obtain high-quality graphene thin sheets. They are based on very different physicochemical processes. Here we demonstrate a novel one step and simple electrografting acrylate monomer method to exfoliate highly oriented pyrolytic graphite (HOPG) into thin nanoplatelets and even down to the single graphene sheet level. Among the high research activity in the area of surface modification, electrografting is a very powerful method which has received comparatively little attention. This is surprising because this technique has many attractive features for modification of conducting or semi-conducting surfaces. The main interest of the electrografting process is to solve the recurrent problem of the organic/substrates interface weakness. The electrografting warranties a robust polymer/substrates interface and offers the possibility to tailor the functionality of the grafted polymer film opening the door to a wide range of demanding technological applications. The graphene sheets obtained through electrografting process give a stable suspension in dimethyl formamide (DMF), and they can self-precipitate on the surface of substrates after adding water as an antisolvent due to their strong surface hydrophobicity. Interestingly, the continuous films obtained exhibit ultratransparency (∼98% transmittance), and the lateral size of the exfoliated graphene sheets observed by AFM ~1nm. Raman and TEM characterizations corroborate that the graphene sheets exfoliated by our electrochemical method preserve the intrinsic structure of grapheme and give preferentially monolayered graphene sheets. The electrochemical behaviour of the acrylate monomer grafted graphene sheets was evaluated in lithium-half cells with no addition of conductive additive or binder. The PAN grafted graphene dispersed in DMF was coated on Cu foil and dried in a vacuum oven at 55°C for 12h. After 200 cycles, the reversible capacity was still kept at 300mAh/g at the current density of 50mA/g. These results indicate that the prepared high quality graphene sheets possess good electrochemical performances for lithium storage. This work provides an efficient approach to obtain high-quality, cost-effective, and scalable production of “graphene ink”, which may pave a way toward future applications in lithium- ion batteries. [less ▲]

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See detailCarbon nanotubes/polypropylene nanocomposites foams for EMI shielding applications
Tran, Minh Phuong ULg; Detrembleur, Christophe ULg; Thomassin, Jean-Michel ULg et al

Conference (2013, September 12)

In order to reduce the undesired effect of the electromagnetic interference, the developing of the materials with high capacity of electromagnetic interference (EMI) shielding has attracted a great ... [more ▼]

In order to reduce the undesired effect of the electromagnetic interference, the developing of the materials with high capacity of electromagnetic interference (EMI) shielding has attracted a great attention to scientific and industrial communities during last two decades.Indeed, polymer carbon nanotubes (CNTs) nanocomposites foams are addressed due to their high electrical conductivity and a great potential applications in electrostatic dissipation (ESD) and in electromagnetic interferences (EMI) shielding. However, the shortcoming of the addition of CNTs is that it usually leads to an increase of permittivity which results in enhancing undesirably the electromagnetic reflectivity due to the mismatch between the wave impedances for the signal propagating into air and into the absorbing material, respectively. To solve this problem, the introduction of air into these nanocomposites by the formation of foam will be favorable in order to reduce the permittivity of conductive composites. A good understanding of the influence of the foam structural parameters on the electrical properties of the foam will ultimately enable the optimum design of these materials for the targeted applications. A wide range of poly (propylene)/CNTs nanocomposites foams were synthesized using the supercritical CO2 technology. Different foaming parameters, such as the temperature, impregnation pressure will be controlled to modify the foam structure. Nanocomposite foams show higher electrical conductivity than non-foamed nanocomposites at the same volume content of CNTs. Effects of foam morphology such as cell density, pore size, volume expansion, and cell-wall thickness on electrical conductivity were comprehensively assessed. Similarly to our previous study on PMMA foam nanocomposites, the electrical conductivity of foams show higher value when the volume expansion is increased and when the average pore size is decreased. The preliminary EMI performances have highlighted that PP/CNTs foams containing 0.1 vol%CNTs are able to absorb about 90% of the incident radiation in the 25 to 40 GHz frequency range. [less ▲]

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See detailMorphology and electrical conductivity of poly(propylene)/multi-walled carbon nanotubes nanocomposites foams compatibilized by poly(propylene) -graft-maleic anhydride (PP-g-MA)
Tran, Minh Phuong ULg; Detrembleur, Christophe ULg; Alexandre, Michaël et al

Poster (2013, September 09)

The agglomerate of carbon nanotubes (CNTs) in poly(propylene) (PP) matrix often results in low electrical conductivity and poor mechanical properties. In order to improve the dispersion of CNTs, different ... [more ▼]

The agglomerate of carbon nanotubes (CNTs) in poly(propylene) (PP) matrix often results in low electrical conductivity and poor mechanical properties. In order to improve the dispersion of CNTs, different amounts of compatibilizer based on poly(propylene-graft-maleic anhydride) (PP-g-MA) were added in the PP matrix. Carbon nanotubes materbatches pre-dispersed at a high loading in the compatibilizer were used to create the samples used in this study. The nanocomposites of PP/PP-g-MA/CNTs were then foamed in supercritical carbon diozide (scCO2) followed by analysis of the foam morphology and the electrical conductivity. The presence of PPgMA did not significantly change the foam morphology, which exhibits good homogeneity and highly uniform closed-cells with penta-heptagonal cell-form. The expansion volume of the foams is not adversely affected by the addition of the compatibilizer; very high expansion volume (around 15 - 25 times) was achieved. The most interesting point is that the PP-PPgMA - 4wt%CNTs foams show a significantly higher electrical conductivity than the uncompatibilized PP-4wt%CNTs at the same volume percent content of CNTs [less ▲]

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See detailElectrografting onto ITO substrates of poly(thiophene)-based micelles decorated by acrylate groups
Ouhib, Farid ULg; Desbief, Simon; Lazzaroni, Roberto et al

in Polymer Chemistry (2013), 4(15), 4151-4161

We report on a simple process for the chemisorption of poly(thiophene)-based block copolymers onto ITO substrates. Two poly(thiophene) block copolymers functionalized by acrylates on the second block are ... [more ▼]

We report on a simple process for the chemisorption of poly(thiophene)-based block copolymers onto ITO substrates. Two poly(thiophene) block copolymers functionalized by acrylates on the second block are prepared by the Grignard Metathesis (GRIM) process. The first block is composed of poly(3-hexylthiophene) (P3HT) and the second block is either a polythiophene bearing an acrylate group on each monomer unit (PAcET), or a polythiophene bearing both acrylate and poly(ethylene glycol) side chains (P(AcET-co-PEGET)). After characterizing their macromolecular parameters and optical properties, we investigate their ability to self-assemble into micelles in DMF solutions. This solvent is required for the electrografting procedure that is used for strongly anchoring the polymer to ITO. These micelles are expected to be formed by a P3HT core and a PAcET or P(AcET-co-PEGET) shell. When PEG side chains are present in the second block, the copolymer nicely self-assembles into micelles decorated by acrylates. Cathodic polarization of ITO induces chemisorption and polymerization of acrylate groups, leading to an adherent organized film of poly(thiophene)-based micelles. The optical absorption spectra show that the electrografted polymer chains have a degree of π-electron conjugation similar to that of crystalline P3HT films. In the absence of the PEG chains, the copolymer does not organize into micelles, due to the low stabilizing ability of the second block in DMF. [less ▲]

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See detailPolymer/carbon based composites as electromagnetic interference (EMI) shielding materials
Thomassin, Jean-Michel ULg; Jérôme, Christine ULg; Pardoen, Thomas et al

in Materials Science & Engineering : R (2013), 74(7), 211-232

The extensive development of electronic systems and telecommunications has lead to major concerns regarding electromagnetic pollution. Motivated by environmental questions and by a wide variety of ... [more ▼]

The extensive development of electronic systems and telecommunications has lead to major concerns regarding electromagnetic pollution. Motivated by environmental questions and by a wide variety of applications, the quest for materials with high efficiency to mitigate electromagnetic interferences (EMI) pollution has become a mainstream field of research. This paper reviews the state-of-the-art research in the design and characterization of polymer/carbon based composites as EMI shielding materials. After a brief introduction, in Section 1, the electromagnetic theory will be briefly discussed in Section 2 setting the foundations of the strategies to be employed to design efficient EMI shielding materials. These materials will be classified in the next section by the type of carbon fillers, involving carbon black, carbon fiber, carbon nanotubes and graphene. The importance of the dispersion method into the polymer matrix (melt-blending, solution processing, etc.) on the final material properties will be discussed. The combination of carbon fillers with other constituents such as metallic nanoparticles or conductive polymers will be the topic of Section 4. The final section will address advanced complex architectures that are currently studied to improve the performances of EMI materials and, in some cases, to impart additional properties such as thermal management and mechanical resistance. In all these studies, we will discuss the efficiency of the composites/devices to absorb and/or reflect the EMI radiation. [less ▲]

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See detailDesign of well-defined N-vinylamides based copolymers via organometalllic-mediated radical polymerization
Debuigne, Antoine ULg; Kermagoret, Anthony ULg; Fustin, Charles-André et al

Conference (2013, June 19)

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See detailEffect of head-to-head addition in vinyl acetate controlled radical polymerization: why is Co(acac)2-mediated polymerization so much better?
Morin, Aurélie N.; Detrembleur, Christophe ULg; Jérôme, Christine ULg et al

in Macromolecules (2013), 46(11), 4303-4312

The controlled polymerization of vinyl acetate has been recently achieved by several techniques, but PVAc with targeted Mn and low dispersity up to very high monomer conversions and high degrees of ... [more ▼]

The controlled polymerization of vinyl acetate has been recently achieved by several techniques, but PVAc with targeted Mn and low dispersity up to very high monomer conversions and high degrees of polymerization was only obtained with Co(acac)2 as controlling agent in the so-called CMRP, a type of organometallic mediated radical polymerization (OMRP). Other techniques (including ATRP, ITP, TERP, and RAFT/MADIX) have shown a more or less pronounced slowdown in the polymerization kinetics, which was attributed to the higher strength of the C−X bond between the radical PVAc chain and the trapping agent (X) in the dormant species and to a consequent slower reactivation after a less frequent head-to-head monomer addition. The reason for the CMRP exception is clarified by the present contribution. First, a detailed investigation by 1H, 13C and multiplicity-edited HSQC and DEPT-135 NMR of the PVAc obtained by CMRP, in comparison with a regular polymer made by free radical polymerization under the same conditions, has revealed that Co(acac)2 does not significantly alter the fraction of head-to-head sequences in the polymer backbone and that there is no accumulation of Co(acac)2-capped chains with a head-to-head ω end. Hence, both dormant chains (following the head-to-head and the head-to-tail monomer additions) must be reactivated at similar rates. A DFT study shows that this is possible because the dormant chains are stabilized not only by the C−Co σ bond but also by formation of a chelate ring through coordination of the ω monomer carbonyl group. The head-to-head dormant chain contains an inherently stronger C−Co bond but forms a weaker 6-membered chelate ring, whereas the weaker C−Co bond in the head-to-tail dormant chain is compensated by a stronger 5-membered chelate ring. Combination of the two effects leads to similar activation enthalpies, as verified by DFT calculations using a variety of local, gradient-corrected, hybrid and “ad hoc” functionals (BPW91, B3PW91, BPW91*, M06 and M06L). While the BDE(C−X) of model H-VAc−X molecules [X = Cl, I, MeTe, EtOC(S)S and Co(acac)2] are functional dependent, the BDE difference between head-to-head and head-to-tail dormant chain models is almost functional insensitive, with values of 5−9 kcal/mol for the ATRP, ITP and TERP models, 3−6 for the RAFT/MADIX model, and around zero for CMRP. [less ▲]

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See detailThe influence of foam morphology of multi-walled carbon nanotubes/poly(methyl methacrylate) nanocomposites on electrical conductivity
Tran, Minh Phuong ULg; Detrembleur, Christophe ULg; Alexandre, Michaël ULg et al

in Polymer (2013), 54(13), 3261-3270

Polymer/multi-walled carbon nanotubes (PMMA/MWNTs) nanocomposites foams are widely investigated during the last decade thanks to their potential applications as electromagnetic interferences shielding ... [more ▼]

Polymer/multi-walled carbon nanotubes (PMMA/MWNTs) nanocomposites foams are widely investigated during the last decade thanks to their potential applications as electromagnetic interferences shielding (EMI) materials. Electrical conductivity of the nanocomposite is a key parameter for these applications. In the frame of this work, we aim at establishing relationships between the foams morphology and their electrical conductivity. We therefore first design nanocomposite foams of various morphologies using supercritical carbon dioxide (scCO2) as physical foaming agent. The nanocomposites based on poly(methyl methacrylate) (PMMA) and different carbon nanotubes loadings are prepared by melt-mixing and foamed by scCO2 in various conditions of pressure, temperature and soaking time. The influence of these foaming conditions on the morphology of the foams (volume expansion, pore size, cell density, cell-wall thickness) is discussed. After measuring the electrical conductivity of the foams, we establish structure/properties relationships that are essential for further optimizations of the materials for the targeted application. [less ▲]

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See detailOne-pot controlled synthesis of double thermoresponsive N-vinylcaprolactam-based copolymers with tunable LCSTs
Kermagoret, Anthony ULg; Fustin, Charles-André; Bourguignon, Maxime et al

in Polymer Chemistry (2013), 4(8), 2575-2583

N-Vinylcaprolactam (NVCL) was copolymerized statistically for the first time in a controlled manner with hydrophilic N-vinylamide or hydrophobic vinylester monomers in order to precisely tune up and down ... [more ▼]

N-Vinylcaprolactam (NVCL) was copolymerized statistically for the first time in a controlled manner with hydrophilic N-vinylamide or hydrophobic vinylester monomers in order to precisely tune up and down the lower critical solution temperature (LCST) of the resulting copolymers. The incorporation of these segments in complex architectures was also considered. Several narrowly distributed NVCL-based copolymers were prepared by cobalt-mediated radical polymerization (CMRP) using the bis-(acetylacetonato)cobalt(II) complex as a controlling agent and N-methyl-N-vinylacetamide (NMVA), N-vinylacetamide (NVA), vinyl acetate (VAc) or vinyl pivalate (VPi) as comonomers. PNVCL-containing block copolymers having two discrete LCSTs were also synthesized following a one-pot strategy based on the sequential CMRP of NVCL followed by the copolymerization of NMVA with the residual NVCL. Upon gradual heating of aqueous solutions of such double thermoresponsive copolymers, we noticed a transition from free chains to micelles before full dehydration and collapse of the block copolymers. These advances represent a significant step towards the development of a platform based on thermoresponsive PNVCL copolymers with a single phase separation or multistep assembly behaviors. [less ▲]

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See detailIn situ nitroxide-mediated polymerization of styrene promoted by the N-tert-butyl-alpha-isopropylnitrone/BPO pair: ESR investigations
Detrembleur, Christophe ULg; Clément, Jean-Louis; Sciannaméa, Valérie et al

in Journal of Polymer Science. Part A, Polymer Chemistry (2013), 51(8), 1786-1795

The styrene polymerization initiated by benzoyl peroxide (BPO) in the presence of N-tert-butyl--isopropylnitrone as nitroxide precursor is well-controlled provided that a prereaction between the nitrone ... [more ▼]

The styrene polymerization initiated by benzoyl peroxide (BPO) in the presence of N-tert-butyl--isopropylnitrone as nitroxide precursor is well-controlled provided that a prereaction between the nitrone and BPO is carried out in suitable conditions prior to polymerization at a higher temperature. Electron spin resonance (ESR) spectroscopy was implemented to probe the nitroxides formed during both steps, that is, the prereaction and polymerization, and to get crucial information regarding the structure of the nitroxides responsible for the polymerization control. ESR studies combined with first principles calculations have evidenced that nitroxides observed during the prereaction in the presence of styrene and during the polymerization steps consist of a mixture of two macronitroxides. One is formed by the addition of a growing polystyrene chain to the nitrone as would be expected. However, the second one results from the addition of a polystyrene chain to tert-butyl nitroso that is in situ formed presumably by decomposition of the first macronitroxide type. [less ▲]

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See detailMagnetic hybrid materials for triggered drug delivery and optical properties of intraocular lens
Liu, Ji ULg; Jérôme, Christine ULg; Detrembleur, Christophe ULg et al

Conference (2013, March 20)

Mesoporous silica nanoparticles have great potential for drug delivery system (DDS) due to their large volume for encapsulation of guest molecules in the porous channels. Due to the specific magnetic ... [more ▼]

Mesoporous silica nanoparticles have great potential for drug delivery system (DDS) due to their large volume for encapsulation of guest molecules in the porous channels. Due to the specific magnetic responsiveness, magnetic nanoparticles can penetrate body tissues under a magnetic guidance, providing a potential platform for magnetic-directed DDS. Furthermore, a sharp local heating can be obtained for superparamagnetic nanoparticles when exposed to an alternating magnetic field (AMF). This specific property opens up the possibility of the application in tumor treatments. Here, we fabricated maghemite/SiO2 mesoporous nanohybrids DDS with phase-changed molecules as gate-keepers. The channels were envisaged to be closed in the biological systems during the delivery; however, opened when exposed to external heating or internal heating from hyperthermia generated by the maghemite cores. Thus the uploaded drug can diffuse into the surrounding medium. MTS assay showed a good cytocompatibility of the vehicles in both mouse L929 cells and cancer MEL-5 cells, and also internalization into MEL-5 cells was confirmed by Fluoresce microscopy, fluoresce-activated cell sorting (FACS) and TEM techniques. The release of drugs can be controlled by varying the concentration of the nanohybrids vehicles, the period of AMF treatment, or both. In-vivo triggered-release of doxorubicin into MEL-5 cells was confirmed by the sharp decrease in cell viability. This DDS can be designed for controlled release to an urgent physiological need via chemotherapy, hyperthermia therapy, or both. [less ▲]

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See detailThermally stable bulk heterojunction solar cells based on cross-linkable acrylate-functionalized polythiophene diblock copolymers
Ouhib, Farid ULg; Tomassetti, Mirco ULg; Manca, Jean et al

in Macromolecules (2013), 46(3), 785-795

We report on the synthesis of new thermally cross-linkable all-conjugated diblock copolymers composed of a poly(3-hexylthiophene) (P3HT) block and an acrylate-functionalized polythiophene block. These ... [more ▼]

We report on the synthesis of new thermally cross-linkable all-conjugated diblock copolymers composed of a poly(3-hexylthiophene) (P3HT) block and an acrylate-functionalized polythiophene block. These copolymers are then used in bulk heterojunction (BHJ) solar cells with [6,6]-phenyl C61-butyric acid methyl ester (PCBM), and their photovoltaic performances are compared with standard P3HT/PCBM devices. Thermal cross-linking of the functional copolymers/PCBM blends is performed to improve the thermal stability of the active layer. BHJ photovoltaic cells with cross-linkable copolymers and PCBM show initial power conversion efficiencies slightly lower than that of P3HT devices. However, solar cells with cross-linkable copolymers retain more than 85% of their initial power efficiency value after 165 h of thermal annealing (accelerated aging test), whereas the same devices with P3HT retain less than 65% of their initial power efficiency. This improvement of the thermal stability of BHJ photovoltaic cells is the result of the polymer network that hampers PCBM diffusion and phase separation, as confirmed with TEM and AFM analysis of the microscopic morphology. Such an improvement is mostly observed when using a cross-linkable P3HT with a short spacer between the acrylate group and the polythiophene backbone. [less ▲]

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