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See detailSpray Drying-­Assisted Synthesis of Na2FePO4F/CB and Na2FePO4F/CNT Composite Cathodes for Lithium Ion Battery
Mahmoud, Abdelfattah ULg; Brisbois; Caes, sebastien et al

Conference (2017, May 08)

Fluorophosphates are considered among the most interesting series of cathode materials for Li/Na-ion batteries. Na2FePO4F, with layered structure and two-dimensional pathways for facile Na+/Li+ transport ... [more ▼]

Fluorophosphates are considered among the most interesting series of cathode materials for Li/Na-ion batteries. Na2FePO4F, with layered structure and two-dimensional pathways for facile Na+/Li+ transport [1], exhibits minimal structural changes (3.7%) upon reduction/oxidation. The average working voltage is 3.3 V versus Li+/Li. However, one of the key drawbacks of Na2FePO4F electrodes is their low intrinsic electronic conductivity. In this work, we report on the synthesis of Na2FePO4F by spray-drying, a technique which is easily scaled-up from the lab- to the industrial-scale and ensures a good homogeneity of all precursors. We are investigating the replacement of the grinding step by the addition of conductive carbon (carbon black and carbon nanotubes) to the solution containing the inorganic precursors of the Na2FePO4F phase in order to prepare Na2FePO4F/CB and Na2FePO4F/CNT with different ratios of CB and CNT (10 and 20%) and enhanced conductivity. The electrochemical performance shows that the addition of CNT improves remarkably the capacity of the NFPF electrode material thanks to better CNT dispersion inside and at the surface of the NFPF particles which enhances the electronic conductivity. Acknowledgements: The authors thank the Walloon Region for support under the “PE Plan Marshall 2.vert” program (BATWAL -1318146). A. Mahmoud is grateful to the Walloon region for a Beware Fellowship Academia 2015-1, RESIBAT n° 1510399. References [1] M. Brisbois, S. Caes, M-T. Sougrati, B. Vertruyen, A. Schrijnemakers, R. Cloots, N. Eshraghi, R-P. Hermann, A. Mahmoud, F. Boschini, Solar Energy Materials & Solar Cells 148 (2015) 11-19. [less ▲]

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See detailSynthesis of hierarchical N-doped porous carbon structure/nanospheres Fe2O3 composites and its application in lithium-ion battery as lithium-ion anodes
Alkarmo, Walid ULg; Ouhib, Farid ULg; Aqil, Abdelhafid ULg et al

Poster (2017, May 04)

Nitrogen-doped porous carbons are of special interest, because their unique physical properties such as high surface area, multidimensional electron transport pathways and good mechanical strength, and ... [more ▼]

Nitrogen-doped porous carbons are of special interest, because their unique physical properties such as high surface area, multidimensional electron transport pathways and good mechanical strength, and are thus very important for applications in the fields of catalysis, environment techniques and energy generation and storage. Moreover, nitrogen-doping can be further amplified in a porous structure that bears a high surface area to increases their materials performance in electrochemical devices, such as double layer capacitors and lithium-ion batteries. In addition, nitrogen-doping can enhance the lithium insertion, between the nitrogen-doped carbon material and lithium. And it can create a large number of defects in the porous configuration and offer more active sites for lithium insertion. Toward this goal, a hierarchically structured macro- and mesoporous N-doped carbon with dispersed Fe2O3 nanoparticles (NDC@Fe2O3) is prepared by thermal treatment of a novel composite composed by PMMA particles decorated by graphene oxide (GO), PPy and iron salts. The NDC@Fe2O3 composite exhibited high surface area with a hierarchical pores structure. Integrated as a lithium ion battery anode, NDC@Fe2O3 exhibited high reversible capacity of 930 mA h/g over 200 cycles. The combination of Fe2O3 nanoparticles with nitrogen-doped porous carbons to form hybrid anode has been an efficient way to maintain the electronic integrity of the whole electrode since the carbon acts as a buffer layer to accommodate the volume variation and to provide multidimensional electron transport pathways during the charge/discharge process. [less ▲]

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See detailUltrasonic spray coating of electrochromic nanomaterials
Maho, Anthony ULg; Manceriu, Laura ULg; Colson, Pierre ULg et al

Conference (2017, May)

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See detailSodium vanadium (III) fluorophosphate/carbon nanotubes composite (NVPF/CNT) prepared by spray-drying: good electrochemical performance thanks to well-dispersed CNT network within NVPF particles
Eshraghi, Nicolas ULg; Caes, Sebastien; Mahmoud, Abdelfattah ULg et al

in Electrochimica Acta (2017), 228

We successfully prepared NASICON-type Na3V2(PO4)2F3 (NVPF) and a Na3V2(PO4)2F3/carbon nanotubes (CNT) composite by spray-drying followed by heat treatment in argon for 2 hours at 600 °C. The addition of ... [more ▼]

We successfully prepared NASICON-type Na3V2(PO4)2F3 (NVPF) and a Na3V2(PO4)2F3/carbon nanotubes (CNT) composite by spray-drying followed by heat treatment in argon for 2 hours at 600 °C. The addition of CNT in the spray-drying solution creates a CNT network within the NVPF particles. After grinding, the smaller NVPF particles remain linked by CNT. Thanks to this conducting network, the composite powder displays competitive electrochemical performance when cycled against lithium in hybrid-ion batteries (2–4.6 V vs. Li+/Li) with specific capacities of 125 mAh.g−1 at C/10, 103 mAh.g−1 at 1C and 91 mAh.g−1 at 4C, together with 97.5% capacity retention at 1C over 100 cycles with coulombic efficiency of 99.4%. These results demonstrate that sodium vanadium (III) fluorophosphate electrode material can be obtained in a time-efficient way using the easily up-scalable spray-drying method. [less ▲]

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See detailComparison of Indium Tin Oxide and Indium Tungsten Oxide as Transparent Conductive Substrates for WO3-Based Electrochromic Devices
Maho, Anthony ULg; Nicolay, Sylvain; Manceriu, Laura ULg et al

in Journal of the Electrochemical Society (2017), 164(2), 25-31

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See detailHydrothermal synthesis of tailored new  promising phosphate particles for lithium and sodium ion batteries
Karegeya, Claude ULg; Mahmoud, Abdelfattah ULg; Sougrati Tahar, Moulay et al

Conference (2016, December 16)

The rechargeable Li-ion batteries dominate the currently used storage systems due to their unrivalled electrochemical properties. However, this technology needs more improvements to meet coast, high ... [more ▼]

The rechargeable Li-ion batteries dominate the currently used storage systems due to their unrivalled electrochemical properties. However, this technology needs more improvements to meet coast, high capacity, safety and environmental requirements. Current researches on Li-ion batteries are focusing on the development of safe and cheap electrode compounds with good electrochemical performance. Iron phosphate-based electrodes have attracted increasing interest due to their environmental compatibility, low cost and its promising electrochemical performance as positive electrode materials in LIB. In this work, we report the electrochemical properties of Fex(PO4)(OH)y.zH2O) cathode material obtained by one-pot hydrothermal synthesis route, a technique which produces the particles with suitable properties for electrode application. We show that the addition of a conducting carbon (carbon black or carbon nanotubes) into the solution has a strong influence on reducing the size and tailoring morphology of material particles. These are among the main factors to enhance the electrochemical performance of the material. Combined with electrochemical and XRD studies, operando Mössbauer analysis shows that Fex(PO4)(OH)y.zH2O) undergoes a reversible reduction/oxidation during lithium intercalation/ deintercalation processes. Acknowledgments This work was supported by the Walloon Region through the BATWAL project [PE Plan Marshall 2.vert]; and the Beware Fellowship Academia [2015-1, RESIBAT n° 1510399]. [less ▲]

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See detailPolyhydroxyurethane hydrogels: synthesis and characterizations
Gennen, Sandro ULg; Grignard, Bruno ULg; Thomassin, Jean-Michel ULg et al

in European Polymer Journal (2016), 84

Hydrogels based on polyurethane (PU) are promising (bio-) materials because of their bio- compatibility, biodegradation and excellent mechanical properties. In this publication, polyurethane hydrogels ... [more ▼]

Hydrogels based on polyurethane (PU) are promising (bio-) materials because of their bio- compatibility, biodegradation and excellent mechanical properties. In this publication, polyurethane hydrogels were produced for the first time by a non-isocyanate route by solvent-free step-growth copolymerization between a CO2-sourced hydrophilic polyethy- lene glycol bi-cyclic carbonate with diamines in the presence of a cross-linker. Kinetic of poly(hydroxyurethane) (PHU) synthesis was monitored by ATR-IR and the chemical cross-linking was confirmed by rheology and gel contents measurements. Hydrogels were obtained by immersion of PHUs in water and the influence of the diamine/cross-linker ratio and the nature of diamine on the water swelling and compression properties (compression modulus, strain and stress at break) of PHU hydrogels was evaluated. Additionally, the compression properties of the hydrogels were improved by the addition of Montmorillonite as nanofiller in the PHU formulation. This work opens new application fields for CO2-sourced PHUs. [less ▲]

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See detailDesign and synthesis of Fe2O3 nanoparticles/N-doped porous carbon structures as high performance electrode for lithium ion battery
Alkarmo, Walid ULg; Ouhib, Farid ULg; Aqil, Abdelhafid ULg et al

Poster (2016, October 13)

Thanks to their fascinating physical properties such as high surface area, multidimensional electron transport pathways and good mechanical strength, three dimensionally (3D) interconnected carbon porous ... [more ▼]

Thanks to their fascinating physical properties such as high surface area, multidimensional electron transport pathways and good mechanical strength, three dimensionally (3D) interconnected carbon porous frameworks have emerged as attractive materials for various electrochemical energy storage/conversion devices, including Li-ion batteries (LIBs), Li−S batteries, supercapacitors and fuel cells. In this context, a hierarchically structured macro- and mesoporous N-doped carbon with dispersed Fe2O3 nanoparticles (NDC@Fe2O3) is prepared by thermal treatment of a novel composite composed by PMMA particles decorated by graphene oxide (GO), PPy and iron salts. The NDC@Fe2O3 composite exhibited high surface area with a hierarchical pores structure. The combination of Fe2O3 nanoparticles with porous carbon to form hybrid anode has been an efficient way to maintain the electronic integrity of the whole electrode since the carbon acts as a buffer layer to accommodate the volume variation and to provide multidimensional electron transport pathways during the charge/discharge process. [less ▲]

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See detailSynthesis and characterization of non-isocyanate polyurethane (NIPU) hydrogels
Gennen, Sandro ULg; Grignard, Bruno ULg; Thomassin, Jean-Michel ULg et al

Poster (2016, October 13)

Due to its good biocompatibility, biodegradation and excellent mechanical properties, polyurethane (PU) is a material of choice for biomedical applications (gloves, tubing, artificial membranes…) and, as ... [more ▼]

Due to its good biocompatibility, biodegradation and excellent mechanical properties, polyurethane (PU) is a material of choice for biomedical applications (gloves, tubing, artificial membranes…) and, as hydrogels, it was used as wound dressing, soft contact lenses, drug delivery systems and scaffolds for tissue engineering. Classically, PU are synthesized by a step-growth polymerization between poly (di-)ols and poly (di-) isocyanates. Due to the toxicity of isocyanates, REACH regulations have changed and, today, there is a need to develop greener and safer route to produce isocyanate-free PUs. This contribution focus on the synthesis of NIPU hydrogels by copolymerizing a bifunctional CO2-sourced hydrophilic PEG bi-cyclic carbonate with diamines in presence of a cross- linker. The PEG bi-cyclic carbonates was prepared via a CO2/epoxide coupling reactions using a new efficient organocatalytic system based on the use of an ammonium salt (TBAI) in combination with a fluorinated alcohol. [less ▲]

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See detailMOSSBAUER SPECTROSCOPY AS A COMPLEMENTARY TECHNIQUE OF X-RAY DIFFRACTION TO INVESTIGATE ELECTRODE MATERIALS FOR ALKALI-ION BATTERIES
Mahmoud, Abdelfattah ULg; sougrati, Moulay Tahar; karegeya, claude et al

Poster (2016, October 09)

Lithium-ion batteries (LIBs) have been widely applied as a power source for portable electronics, stationary energy storage systems, and electric vehicles. Nevertheless, as lithium resources continue to ... [more ▼]

Lithium-ion batteries (LIBs) have been widely applied as a power source for portable electronics, stationary energy storage systems, and electric vehicles. Nevertheless, as lithium resources continue to decline worldwide and Li in the Earth’s crust is unevenly distributed as minor-metal. Na-ion batteries are considered to be an alternative to Li-ion batteries owing to the natural abundance of sodium. Indeed, Sodium-ion (Na-ion) batteries are expected to become part of the mix of technologies that will meet the challenges of energy storage. Electrode materials are the most important components in the operation and the performances of Alkali-ion batteries. New electrode materials are required to increase the energy density of Li/Na-ion batteries [1]. Fe based negative electrode materials for Li-ion batteries have been previously investigated to evaluate the electrochemical performances and elucidate the electrochemical reaction mechanisms. Mössbauer spectroscopy has been applied to a variety of fields including chemistry, physics, geology, biology…. In the domain of energy storage, Mössbauer spectroscopy has been used as a powerful tool to investigate the local electronic and structural properties of electrode materials and to determine their reaction mechanisms during charge and discharge of Li/Na-ion batteries [2]. In this poster, we will show from some selected examples how Mössbauer spectroscopy when used with X-ray diffraction can help to improve the performances of electrode materials for Alkali-ion batteries. References 1. Sougrati MT, Darwiche A, Liu X, Mahmoud A, Hermann RP, Jouen S, Monconduit L, Dronskowski R, Stievano L: Transition-metal carbodiimides as molecular negative electrode materials for lithium- and sodium-ion batteries with excellent cycling properties. Angew Chem Int Ed., 2016, 55: 5090-5095. 2. Brisbois, M., Caes, S., Sougrati, M. T., Vertruyen, B., Schrijnemakers, A., Cloots, R., Eshraghi, N., Hermann, R. P., Mahmoud, A., Boschini, F. Na2FePO4F/Multi-Walled Carbon Nanotubes for Lithium-Ion Batteries_ Operando Mössbauer Study of Spray- Dried Composites. Solar Energy Materials and Solar Cells 2016, 148, 67–72. Acknowledgment A. Mahmoud and F. Boschini would like to kindly thank Wallonie regions for the financial support. [less ▲]

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See detailPhosphate-based composite electrodes for Li/Na-ion batteries: upscalable solution syntheses with in-situ solid carbon addition
Vertruyen, Bénédicte ULg; Brisbois, Magali; Eshraghi, Nicolas ULg et al

Conference (2016, September 22)

Since the success story of lithium iron phosphate, other phosphate-based compounds have attracted a lot of interest as promising candidates for positive electrodes in lithium-ion or sodium-ion batteries ... [more ▼]

Since the success story of lithium iron phosphate, other phosphate-based compounds have attracted a lot of interest as promising candidates for positive electrodes in lithium-ion or sodium-ion batteries. Their electronic conductivity usually has to be improved through the preparation of composite powders ensuring intimate contact between the active material and conductive carbon. We report on the one-step synthesis of composite precursors using spray-drying or hydrothermal synthesis routes, two techniques which offer easy scaling-up of production. We show that addition of a solid carbon source (carbon black or carbon nanotubes) into the solution has a strong influence on the powder microstructure and is very effective in improving the battery cycling performance, taking our recent results on phosphates [Fex(PO4)(OH)y.zH2O)] and fluorophosphates [Na2FePO4F, Na3V2(PO4)2F3] as examples. We also compare this approach with the addition of the carbon source as a soluble precursor (such as ascorbic acid or citric acid) where the in situ formation of carbon is achieved by a heat treatment in inert atmosphere (typically argon). [less ▲]

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See detailSynthesis and characterizations of non-isocyanate polyurethane (NIPU) hydrogels
Gennen, Sandro ULg; Grignard, Bruno ULg; Thomassin, Jean-Michel ULg et al

Poster (2016, September 12)

Polyurethane (PU) is on of the most used polymers for the preparation of hydrogels due to its good biocompatibility, biodegradation and excellent mechanical properties. PU hydrogels are found in lot of ... [more ▼]

Polyurethane (PU) is on of the most used polymers for the preparation of hydrogels due to its good biocompatibility, biodegradation and excellent mechanical properties. PU hydrogels are found in lot of applications such as wound dressing, soft contact lenses, drug delivery and scaffolds for tissue engineering. Classicaly, PU is produced by a step-growth polymerization between diols and diisocyanates. However, in order to avoid the use of harmful isocyanates compounds and because of regulations which tend to ban the use of isocyanates, we developed hydrogels based on a non-isocyanate polyurethane (NIPU) chemistry by valorizing CO2-sourced cyclic carbonates and amines. Precisely, NIPU hydrogels were prepared by a solvent-free copolymerization between bifunctional hydrophilic polyethylene glycol cyclic carbonates and diamines in presence of a triamine as a crosslinker, followed by a water swelling of the obtained cross-linked gel. Parameters such as the cross-linking ratio and diamine’s nature were optimized. Different clay contents (cloiste 30B) as nanofiller were dispersed in the ideal cyclic carbonate/diamine/triamine formulation prior polymerization in order to reinforce the compression properties of NIPU hydrogels. Finaly, we were able to prepare NIPU hydrogels with water content up to 80 % and good compression properties using low clay content. [less ▲]

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See detailValorization of CO2 for the preparation of advanced materials
Gennen, Sandro ULg; Grignard, Bruno ULg; Thomassin, Jean-Michel ULg et al

Conference (2016, July 07)

Detailed reference viewed: 29 (6 ULg)
See detailFe2O3 nanoparticle-functionalized N-doped carbon with interconnected, hierarchical porous structures as high-performance electrode for lithium ion batteries
Alkarmo, Walid ULg; Ouhib, Farid ULg; Aqil, Abdelhafid ULg et al

Poster (2016, May 23)

Thanks to their fascinating physical properties such as high surface area, multidimensional electron transport pathways and good mechanical strength, three dimensionally (3D) interconnected carbon porous ... [more ▼]

Thanks to their fascinating physical properties such as high surface area, multidimensional electron transport pathways and good mechanical strength, three dimensionally (3D) interconnected carbon porous frameworks have emerged as attractive materials for various electrochemical energy storage/conversion devices, including Li-ion batteries (LIBs), Li−O2 batteries, Li−S batteries, supercapacitors, and fuel cells. A hierarchically structured macro- and mesoporous N-doped carbon with dispersed Fe2O3 nanoparticles (NDC@Fe2O3) is prepared by thermal treatment of a novel composite composed by PMMA particles decorated by graphene oxide (GO), PPy and iron salts. The NDC@Fe2O3 composite exhibited high surface area with a hierarchical pores structure. Integrated as a lithium ion battery anode, NDC@Fe2O3 exhibited high reversible capacity of 930 mA h/g over 200 cycles. The combination of Fe2O3 nanoparticles with porous carbon to form hybrid anode has been an efficient way to maintain the electronic integrity of the whole electrode since the carbon acts as a buffer layer to accommodate the volume variation and to provide multidimensional electron transport pathways during the charge/discharge process. [less ▲]

Detailed reference viewed: 370 (12 ULg)
See detailSynthesis of CO2-sourced hydrogels by using the non-isocyanate polyurethane (NIPU) chemistry
Gennen, Sandro ULg; Grignard, Bruno ULg; Thomassin, Jean-Michel ULg et al

Poster (2016, May 23)

Polyurethane (PUs) is one of the most important polymers and finds applications as elastomers, coatings, adhesives and sealants for automotive or construction. PU is also a material of choice in the ... [more ▼]

Polyurethane (PUs) is one of the most important polymers and finds applications as elastomers, coatings, adhesives and sealants for automotive or construction. PU is also a material of choice in the biomedical domain due to its good biocompatibility, biodegradation and mechanical properties. Especially, PUs hydrogels have been developed in the last years for biomedical applications such as soft contact lenses, wound dressing, drug delivery systems and scaffolds for tissue engineering. Traditionally, PUs are synthesized by a step-growth polymerization between diols and diisocyanates. Because of toxicity issues and a possible interdiction of isocyanates, we focused on developing new PU hydrogels using a non-isocyanate route (Figure 1). The polyurethanes formed by this route are called NIPU (for Non-Isocyanate PolyUrethane). Firstly, chemically cross-linked NIPU gels were synthesized by solvent-free polycondensation between a hydrophilic CO2-sourced polyethyleneglycol bi-cyclic carbonate and a diamine in the presence of a crosslinker. Then, NIPU gels were swelled in water till water equilibrium before characterization of their mechanical properties by compression tests. The influence of the cross-linking ratios (diamine/crosslinker ratio) and diamine structure on the swelling and the compression properties were studied. To reinforce the compression properties of NIPU hydrogel (increase in stress at break, strain at break and compression modulus), a nanofiller was dispersed in the cyclic carbonate/diamine/crosslinker formulation prior to polymerization. For the first time, nanocomposite NIPU hydrogels with high water contents (up to 80%) and good compression properties have been prepared by using low clay content. [less ▲]

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See detailOn the Habitability of Desert Varnish: a Combined Study by Micro-Raman Spectroscopy, X-Ray Diffraction and Methylated Pyrolysis-Gas Chromatography-Mass Spectrometry
Malherbe, Cédric ULg; Hutchinson, Ian; Ingley, Richard et al

in Astrobiology (2016)

In 2020, the ESA ExoMars and NASA Mars 2020 missions will be launched to Mars, searching for evidence of past and present life. In preparation for these missions, terrestrial analogue samples of rock ... [more ▼]

In 2020, the ESA ExoMars and NASA Mars 2020 missions will be launched to Mars, searching for evidence of past and present life. In preparation for these missions, terrestrial analogue samples of rock formations on Mars are studied in detail in order to optimize the scientific information that the analytical instrumentation will return. Desert varnishes are thin mineral coatings found on rocks in arid and semi-arid environments on Earth that are recognized as analogue samples. During the formation of desert varnishes (which takes many hundreds of years) organic matter is incorporated and microorganisms may also play an active role in the formation process. During this study, four complementary analytical techniques proposed for Mars missions (X-rays diffraction, Raman spectroscopy, elemental analysis and pyrolysis-gas chromatography-mass spectrometry) were used to interrogate samples of desert varnish and to describe their capacity to sustain life under extreme scenario. For the first time, both the geochemistry and the organic compounds associated with desert varnish are described using an identical set of samples. XRD and Raman spectroscopy measurements were used to non-destructively interrogate the mineralogy of the samples. In addition, the use of Raman spectroscopy instruments enabled the detection of β-carotene, a highly Raman active biomarker. The content and the nature of the organic material in the samples was further investigated using elemental analysis and methylated Py-GC-MS and a bacterial origin was determined to be likely. In the context of planetary exploration, we describe the habitable nature of desert varnish based on the bio-geochemical composition of the samples. Possible interference of the geological substrate on the detectability of pyrolysis products is also suggested. [less ▲]

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