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See detailSpray-drying as a versatile synthesis method for fluorophosphate-based compounds as cathodes material for Na-ion batteries
Bodart, Jérôme ULiege; Eshraghi, Nicolas ULiege; Mahmoud, Abdelfattah ULiege et al

Conference (2019, July 22)

Fluorophosphate compounds attract much attention as cathode materials for Na-ion batteries. Indeed, thanks to the inductive effect of the fluoride and phosphate groups, such compounds exhibit a relatively ... [more ▼]

Fluorophosphate compounds attract much attention as cathode materials for Na-ion batteries. Indeed, thanks to the inductive effect of the fluoride and phosphate groups, such compounds exhibit a relatively high working potential and good theoretical capacity [1]. In this work, we focus on the iron (Na2FePO4F (NFPF)) and vanadium (Na3V2(PO4)3F3 (NVPF)) based fluorophosphate materials which are characterized by a high theoretical capacity of 124 mAh/g and 128 mAh/g, respectively. In addition, the iron-based phase is also more environmental friendly due to the low toxicity of the iron. The preparation of such complex phases using conventional solid-state route requires at least two steps with long heat treatment durations. Here, we report a facile aqueous synthesis using the spray-drying method that can be used for both NFPF and NVPF materials and that can be tuned in order to optimize the composition and the morphology of the desired materials. The major limitation of phosphate-based electrodes is their low intrinsic electronic conductivity. The synthesis of composites with carbon is an effective strategy for the enhancement of the electronic conductivity of these compounds. Spray-drying is a suitable method to incorporate carbon in composite compounds due to the high homogeneity of the obtained particle [2]. It is also a cost effective and up-scalable technique which can produce large quantities of the desired material. Here, we report the influence of the carbon addition on the structural, morphological and electrochemical properties of NFPF and NVPF compounds. The prepared composite materials were investigated by combining several characterisation techniques such as XRD, SEM and TEM. The electrochemical properties were evaluated by galvanostatic cycling and electrochemical impedance spectroscopy in Na-ion batteries. [less ▲]

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See detailBlack phosphorus-based polyvinylidene fluoride nanocomposites: Synthesis, processing and characterization
Tiouitchi, Ghassane; Raji, Marya; Mounkachi, Omar et al

in Composites Part B: Engineering (2019), 175

In this study, the polyvinylidene fluoride (PVDF) nanocomposites were produced based on the few-layers Black phosphorus nanosheets (BP) via the liquid exfoliation method, and at different BP nanofiller ... [more ▼]

In this study, the polyvinylidene fluoride (PVDF) nanocomposites were produced based on the few-layers Black phosphorus nanosheets (BP) via the liquid exfoliation method, and at different BP nanofiller contents (1, 2.5 and 5 wt%). A masterbatch with 5 wt% of BP was prepared by solution blending followed by melt compounding process to elaborate the different nanocomposites and compression molding to molding all samples. The characterization of the nanocomposites in terms of X-ray diffraction, infrared spectroscopy, and scanning electron microscopy confirmed that BP nanosheets were successfully prepared. The nanocomposites were characterized in terms of structural, thermal, electrical, and mechanical performances. The thermal stability of neat PVDF was found increased with 5 wt% of BP nanofillers addition. For the same concentration, the electrical conductivity was sharply increased from 3.3 e−14 to 5 e−11 S/cm. Similarly, Young's modulus value was found increased by 56% as compared to the neat matrix. BP nanofillers appear to be a good alternative to elaborate new polymer nanocomposites with improved performances. [less ▲]

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See detailXPS and Raman study of spray-dried Na3V2(PO4)2F3/C as cathode material for sodium ion batteries
Eshraghi, Nicolas ULiege; Bodart, Jérôme ULiege; Mahmoud, Abdelfattah ULiege et al

Poster (2019, May 28)

Na3V2(PO4)2F3 (NVPF) has attracted much attention as cathode material for Na-ion batteries thanks to the inductive effects allowing for a high working potential combined with a high theoretical specific ... [more ▼]

Na3V2(PO4)2F3 (NVPF) has attracted much attention as cathode material for Na-ion batteries thanks to the inductive effects allowing for a high working potential combined with a high theoretical specific capacity due to the multiple oxidation states of vanadium [1-2]. One of the limitations of NVPF electrodes is their low intrinsic electronic conductivity; therefore, we have prepared composites of NVPF with conductive carbon sources to ensure higher electronic conductivity of the electrodes. NVPF and NVPF/carbon composite materials were prepared by spray-drying as in our previous work [2]. Spray drying is a cost-effective and up-scalable route to prepare homogeneous multi-component powders, thus making it a suitable method to incorporate carbon in the composite powder [4]. The influence of different carbon sources on structural and morphological properties of NVPF and NVPF/carbon composite was investigated by combining several characterization techniques (XRD, SEM and TEM). The chemical composition at the surface of the powders were studied using XPS. Raman spectroscopy was used to evaluate the quality in disordered carbon materials and its electronic conductivity [3] and compare the results with the results from EIS and cycling performance of different samples. References: [1] Shakoor et al., Chem. 22,2012, 20535. [2] Eshraghi et al., Electrochimica Acta, 228, 2017, 319. [3] Mahmoud et al., J Solid State Electrochem. 22, 2018,103. [4] Vertruyen et al., Materials 2018, 11, 1076. [less ▲]

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See detailElectrode materials for Li-ion and Na-ion batteries prepared by hydrothermal and spray drying methods
Mahmoud, Abdelfattah ULiege; Bodart, Jérôme ULiege; karegeya, claude et al

Conference (2019, May 21)

Li-ion batteries are widely used energy storage; however they are limited by availability of materials, price and safety. Regarding economic reasons and preservation of Earth resources, it is necessary to ... [more ▼]

Li-ion batteries are widely used energy storage; however they are limited by availability of materials, price and safety. Regarding economic reasons and preservation of Earth resources, it is necessary to anticipate the lithium substitution by more abundant elements. Sodium-ion batteries are potential candidates to replace Li-ion batteries because the sodium sources are “unlimited”, attainable at low-cost, and geographically distributed. The electrode materials optimization plays a key role in the development of advanced rechargeable batteries. Indeed, the electrode properties have a great influence on the safety, performance and durability of alkali-ion batteries [1]. Spray-drying and hydrothermal (solvothermal) methods are very appropriate to obtain electrode materials for alkali-ion batteries [2-4]. Both techniques are easily adaptable to new materials and can be applied to a wide range of potential electrode materials. These two synthesis methods, suitable for a large-scale industrial production, allow forming spherical aggregates at low temperatures. A variety of synthetic conditions can be tested including different calcination temperatures, dilution of the starting slurry, milling the material in the dry state and in various nonaqueous solvents. In addition, it is possible to mix the precursors with conductive additives during the material synthesis, leading to carbon/active material composites blends at the nanometric level [3]. In this presentation, we report the synthesis and the study of the iron-based phosphate materials (Na1.25Ni1.25Fe1.75(PO4)3, Na2Mn1.5Fe1.5(PO4)3 [4], Na2FePO4F...) for Li/Na-ion batteries. Mössbauer spectroscopy analyses was combined with other characterization techniques (X-ray diffraction, SEM, TEM, impedance spectroscopy, etc.) to study and investigate the structural, magnetic and electrochemical properties of electrode materials prepared by spray-drying and hydrothermal synthesis methods. References [1]. N. Yabuuchi, K.Kubota, M. Dahbi, S. Komaba, Chem. Rev. 114 (23) (2014) 11636-11682. [2] B. Vertruyen, N. Eshraghi, C. Piffet, J. Bodart, A. Mahmoud, F. Boschini; Materials 11 (7) (2018) 1076. [3] C. Karegeya, A. Mahmoud, R. Cloots, B. Vertruyen, F. Boschini, Electrochimica Acta 250 (2017) 49-58. [4] C. Karegeya, A. Mahmoud, B. Vertruyen, F. Hatert, R. Cloots, F. Boschini. Solid State Ionics, 312 (2017) 88-96 ACKNOWLEDGMENTS The authors are grateful to the University of Liège and FRS-FNRS for the financial support. Part of this work was supported by the Walloon Region under the “PE PlanMarshall2. vert”program (BATWAL 1318146). A.M. is grateful to the Walloon region for a Beware Fellowship Academia 2015-1,RESIBAT no. 1510399 and University of Liége. [less ▲]

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See detailLarge Magnetic Entropy Change in Pr2/3Sr1/3MnO3-CuO Composite at Room Temperature
Fkhar, L.; Mounkachi, O.; El Maalam, K. et al

in Journal of Superconductivity and Novel Magnetism (2019)

We report in this paper the impact of copper oxide (CuO) on the structural, magnetic, and magnetocaloric properties of Pr2/3Sr1/3MnO3 (PSMO) material. Our samples were synthesized by conventional solid ... [more ▼]

We report in this paper the impact of copper oxide (CuO) on the structural, magnetic, and magnetocaloric properties of Pr2/3Sr1/3MnO3 (PSMO) material. Our samples were synthesized by conventional solid-state reaction. The phase formation with no impurities was verified using the X-ray diffraction (XRD). The magnetic properties measured by Magnetic Properties Measurement System (MPMS) show the impact of the AFM CuO semiconductor on the magnetization and the transition temperature of the composite. The magnetic entropy changes were calculated from the isothermal curve of the magnetization as a function of the magnetic field. It is found that a small amount of copper oxide is enough to enhance the magnetocaloric properties of our materials. [less ▲]

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See detailCO2-sourced polycarbonates as solid electrolytes for room temperature operation lithium battery
Ouhib, Farid; Meabe, Leire; Mahmoud, Abdelfattah ULiege et al

in Journal of Materials Chemistry A (2019), 7(16), 9844-9853

In the last years, polycarbonates have been identified as alternatives to poly(ethylene oxide) as polymer electrolytes for lithium battery applications. In this work, we show the design of CO2-sourced ... [more ▼]

In the last years, polycarbonates have been identified as alternatives to poly(ethylene oxide) as polymer electrolytes for lithium battery applications. In this work, we show the design of CO2-sourced polycarbonates for its use in a room temperature lithium battery. Novel functional polycarbonates alternating oxo-carbonate moieties and polyethylene oxide segments are synthesized by the facile room temperature (rt) organocatalyzed polyaddition of CO2-sourced bis(?-alkylidene carbonate)s (bis-?CCs) with polyethylene oxide diols. The effect of the polyethylene oxide molar mass on the ionic conductivity and on the thermal properties of the poly(oxo-carbonate)s is investigated. The best candidate shows a low glass temperature of -44°C and a high ionic conductivity of 3.75 * 10-5 S cm-1 at rt when loaded with 30 wt% bis(trifluoromethanesulfonyl)imide salt (LiTFSI) without any solvent. All solid semi-interpenetrated network polymer electrolyte (SIN-SPE) is then fabricated by UV-cross-linking of a mixture containing a specifically designed poly(oxo-carbonate) bearing methacrylate pendants, diethylene glycol diacrylate and the previously described poly(oxo-carbonate) containing LiTFSI. The resulting self-standing membrane exhibits a high oxidation stability up to 5 V (vs Li/Li+), an ionic conductivity of 1.1 * 10-5 S cm-1 at rt (10-4 S cm-1 at 60°C) and promising mechanical properties. Assembled in a half cell configuration with LiFePO4 (LFP) as cathode and lithium as anode, the all-solid cell delivers a discharge capacity of 161 mAh g-1 at 0.1C and 60°C, which is very close to the theoretical capacity of LFP (170 mAh g-1). Also, a stable reversible cycling capacity over 400 cycles with high coulombic efficiency of 99 % is noted at 1C. Similar results are obtained at rt provided that 10 wt% of tetraglyme as plastisizer were added to SIN-SPE. I. [less ▲]

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See detailSodium Iron Sulfate Alluaudite Solid Solution for Na-ion Batteries: Moving Towards Stoichiometric Na2Fe2(SO4)3
Jungers, Thomas ULiege; Mahmoud, Abdelfattah ULiege; Malherbe, Cédric ULiege et al

in Journal of Materials Chemistry A (2019), 7

Thanks to the inductive effect of the sulfate groups, sodium iron sulfate alluaudites display the highest electrode potential amongst the Fe-based compounds studied in sodium-ion batteries. Here, we ... [more ▼]

Thanks to the inductive effect of the sulfate groups, sodium iron sulfate alluaudites display the highest electrode potential amongst the Fe-based compounds studied in sodium-ion batteries. Here, we report the synthetic strategy that has allowed us to obtain the elusive Na2Fe2(SO4)3 stoichiometric compound through a reverse-strike coprecipitation method in organic medium. We experimentally confirm the hypothesis that the stoichiometric compound transforms upon further heat treatment into the previously reported sodium-rich solid solution and an iron sulfate secondary phase. X-ray diffraction and 57Fe Mössbauer spectroscopy do not reveal any striking structure difference between the stoichiometric and Na-rich compounds, in agreement with the current understanding that the instability of the stoichiometric phase is due to the repulsion between Fe2+ ions in the Fe2O10 dimers bridged by sulfate groups. Despite less-than-optimal powder microstructure, electrochemical activity of the stoichiometric phase could be demonstrated through operando X-ray diffraction. These findings are expected to shift attention towards the (near)-stoichiometric compositions, which offer the highest theoretical specific capacities thanks to their optimal Na/Fe ratio. [less ▲]

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See detailElectrical and electrochemical properties of Li2M(WO4)2 (M = Ni, Co and Cu) compounds
Karoui, Karim; Mahmoud, Abdelfattah ULiege; Ben Rhaiem, Abdallah et al

in RSC Advances (2019), 9

Li2M(WO4)2 (M = Co, Cu or Ni) materials have been synthesized using the solid-state reaction method. X-ray diffraction measurements confirmed the single phase of the synthesized compounds in the triclinic ... [more ▼]

Li2M(WO4)2 (M = Co, Cu or Ni) materials have been synthesized using the solid-state reaction method. X-ray diffraction measurements confirmed the single phase of the synthesized compounds in the triclinic crystal system (space group P̄). The SEM analyses revealed nearly spherical morphology with the particle size in the range of 1–10 μm. The IR spectra confirm the presence of all modes of WO42−. The impedance spectroscopy measurements showed the presence of grain boundaries and allow determination of the conductivity of the synthesized materials at room temperature. As positive electrode materials for lithium ion batteries, Li2M(WO4)2 (M = Co, Cu or Ni) cathode materials deliver initial discharge capacities of 31, 33 and 30 mA h g−1 for cobalt, nickel, and copper, respectively. [less ▲]

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See detailOptical and AC conductivity studies on Li 2-x Rb x MoO 4 (x = 0, 0.5, 1) compounds
Ben Nasr, Wafa; Mahmoud, Abdelfattah ULiege; Boschini, Frédéric ULiege et al

in Journal of Alloys and Compounds (2019), 788

In this work, we are interested in the new compounds Li 1.5 Rb 0.5 MoO 4 preparation by the solid state method. Also, we present a comparative study with LiRbMoO 4 and Li 2 MoO 4 . The X-ray powder ... [more ▼]

In this work, we are interested in the new compounds Li 1.5 Rb 0.5 MoO 4 preparation by the solid state method. Also, we present a comparative study with LiRbMoO 4 and Li 2 MoO 4 . The X-ray powder diffraction indicates that these compounds crystallize at room temperature in the monoclinic, orthorhombic and trigonal systems with the P2 1 , Pcab and R-3 space groups, respectively. The shapes of the grains for these ceramics were observed by means of scanning electron microscopy (SEM) images. The Tauc model was used to determine the optical gap energy (4, 4.3 and 3.9 ev) and the urbach energies (1.51, 0.35 and 1.14 ev) of our compounds. The electric and dielectric proprieties of Li 1.5 Rb 0.5 MoO 4 have been studied. We carried out complex impedance spectroscopy in the frequency range 200 Hz-5 MHz at different temperatures (575–723 K). The complex impedance diagram showed a single semicircle, implying that the response originates corresponding to the grains. As a result, an electrical equivalent circuit has been proposed. The spectra follow the Arrhenius law with two energies of activation 1.58 eV for impedance measurements and 1.25 eV for that of modulus. The alternative current (AC) electrical conduction of the three compounds is governed by the overlapping large polaron tunneling (OLPT). © 2019 [less ▲]

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See detailHydrothermal synthesis and electrochemical properties of Fe1.19(PO4)(OH)0.57(H2O)0.43/C cathode material for Li-ion batteries
Mahmoud, Abdelfattah ULiege; Karegeya, Claude; Sougrati, Moulay Tahar et al

Conference (2019, January 29)

Recent rapid development of the portable electronic devices, growing interest in the electric vehicles and increasing integration the renewable energies required the development of cost-effective and high ... [more ▼]

Recent rapid development of the portable electronic devices, growing interest in the electric vehicles and increasing integration the renewable energies required the development of cost-effective and high energy storage systems. Lithium-ion batteries are considered as system of the choice for variety of mobile and stationary applications. However, new electrode materials are demanded to increase the energy density of Li-ion batteries. This presentation will report on the preparation and study of Fe1.19(PO4)(OH)0.57(H2O)0.43/C ((FPHH/C) composite as positive electrode material with high capacity and long cycle-life [1, 2]. FPHH/C (C= carbon black (CB) and carbon nanotubes (CNT)) composites were obtained by one-step the hydrothermal synthesis route. These cathode materials showed an excellent reversible capacity corresponding to 1.19 Li reaction. This is attributed to the stable and open structure of FPHH and also to the effect of carbon addition (CB and CNT) that improves the electronic percolation of the composite. The study of the reaction mechanism of FPHH/CNT during cycling by combining operando XRD and 57Fe Mossbauer spectroscopy (Figure 1) shows that the insertion mechanism is a monophasic reaction with 10% volume variations associated to the Fe3+/Fe2+ redox reaction [2]. References 1. C. Karegeya, A. Mahmoud, R. Cloots, B. Vertruyen, F. Boschini. Electrochimica Acta 250 (2017) 49-58. 2. A. Mahmoud, C. Karegeya, M. T. Sougrati, J. Bodart, B. Vertruyen, R. Cloots, P-E. Lippens, F. Boschini. ACS Applied Materials and interfaces 10 (2018) 34202-34211. [less ▲]

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See detailStructural, vibrational spectroscopic, and electrical conduction mechanisms of $\alpha$-NaCoPO4 compound
Ajmi, Asma; Chemingui, Mahmoud; Mahmoud, Abdelfattah ULiege et al

in Ionics (2019), 25(3), 1091--1103

The orthophosphate alpha-NaCoPO4 compound was prepared from highly pure constituents with mechanical milling followed by heat treatment. X-ray diffraction data refined via Rietveld method revealed that ... [more ▼]

The orthophosphate alpha-NaCoPO4 compound was prepared from highly pure constituents with mechanical milling followed by heat treatment. X-ray diffraction data refined via Rietveld method revealed that this compound crystallizes in the orthorhombic system with Pnma space group. A thermal analysis shows that this composition undergoes one-phase transitions at Tþinspace=þinspace567 K. The infrared and Raman spectra confirm the presence of PO43− tetrahedral. The evolution of half-width $\Delta$$\nu$ and intensity report versus temperature introduces huge changes associated with the phase transition originating from the reorientation of the PO4 tetrahedra. Besides, the electrical data analysis of the impedance spectra is adapted to an equivalent circuit. Furthermore, the alternating current (AC) conductivity of grain contribution is interpreted using the Jonscher's universal power law. The AC conductivity behavior is ensured by a single process defined as a hopping transport mechanism. The conductivity frequency dependence is interpreted using the non-overlapping small polaron tunneling model (NSPT) in the two phases. [less ▲]

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See detailAn easy route to synthesize high-quality black phosphorus from amorphous red phosphorus
Tiouitchi, G.; Ali, M. Ait; Benyoussef, A. et al

in Materials Letters (2019), 236

The development of an easy and efficient process for producing black phosphorus (BP) remains a bottleneck for the use of BP in large-scale applications. In this work, we present a simple, potentially ... [more ▼]

The development of an easy and efficient process for producing black phosphorus (BP) remains a bottleneck for the use of BP in large-scale applications. In this work, we present a simple, potentially scalable, and economically viable method for the preparation of high-quality BP from amorphous red phosphorus. BP was synthesized under low pressure and temperature conditions from red phosphorus via the addition of small quantities of copper, tin, and tin(IV) iodide. Characterization by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDX), high-resolution transmission electron microscopy (HR-TEM), and Raman spectroscopy were performed to confirm the high quality and purity of the formed BP. [less ▲]

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See detailStudy of the Structural and Magnetic Properties of Co-Substituted Ba2Mg2Fe12O22 Hexaferrites Synthesized by Sonochemical Co-Precipitation
Koutzarova, Tatyana; Kolev, Svetoslav; Krezhov, Kiril et al

in Materials (2019), 12(9 1414),

Ba2Mg0.4Co1.6Fe12O22 was prepared in powder form by sonochemical co-precipitation and examined by X-ray diffraction, Mössbauer spectroscopy and magnetization measurements. Careful XRD data analyses ... [more ▼]

Ba2Mg0.4Co1.6Fe12O22 was prepared in powder form by sonochemical co-precipitation and examined by X-ray diffraction, Mössbauer spectroscopy and magnetization measurements. Careful XRD data analyses revealed the Y-type hexaferrite structure as an almost pure phase with a very small amount of CoFe2O4 as an impurity phase (about 1.4%). No substantial changes were observed in the unit cell parameters of Ba2Mg0.4Co1.6Fe12O22 in comparison with the unsubstituted compound. The Mössbauer parameters for Ba2Mg0.4Co1.6Fe12O22 were close to those previously found (within the limits of uncertainty) for undoped Ba2Mg2Fe12O22. Isomer shifts (0.27–0.38 mm/s) typical for high-spin Fe3+ in various environments were evaluated and no ferrous Fe2+ form was observed. However, despite the indicated lack of changes in the iron oxidation state, the cationic substitution resulted in a significant increase in the magnetization and in a modification of the thermomagnetic curves. The magnetization values at 50 kOe were 34.5 emu/g at 4.2 K and 30.5 emu/g at 300 K. The zero-field-cooled (ZFC) and field-cooled (FC) magnetization curves were measured in magnetic fields of 50 Oe, 100 Oe, 500 Oe and 1000 Oe, and revealed the presence of two magnetic phase transitions. Both transitions are shifted to higher temperatures compared to the undoped compound, while the ferrimagnetic arrangement at room temperature is transformed to a helical spin order at about 195 K, which is considered to be a prerequisite for the material to exhibit multiferroic properties. [less ▲]

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See detailSynthesis of Na2FePO4F by spray drying in order to optimise the composition and morphology for Na-ion batteries applications
Bodart, Jérôme ULiege; Violle, Denis; Mahmoud, Abdelfattah ULiege et al

Poster (2018, December 13)

Li-ion batteries are well-developed for numerous applications but the limited resources and expensive price of lithium urge the necessity to find a viable alternative to lithium. Na-ion batteries are ... [more ▼]

Li-ion batteries are well-developed for numerous applications but the limited resources and expensive price of lithium urge the necessity to find a viable alternative to lithium. Na-ion batteries are considered as a good alternative to Li-ion batteries due to the abundance and well-distributed presence of sodium on earth crust. It is then necessary to develop new electrode material for sodium batteries, with low cost, high energy density and long cycling life. This work presents the synthesis of Na2FePO4F by spray-drying method. In order to compensate the low conductivity of phosphate based materials, carbon nanotubes (CNT) are added during the preparation of the precursor solution. The solution/suspension is spray-dried to obtain a composite precursor and after calcination the desired phase. The spray-drying technique is appropriate to variate the morphology and to control it by modifying the injection parameters (Pressure, temperature, flow rate, injection nozzle). The addition of carbon nanotubes lead to an undesired reduction of the iron to the metallic state. To resolve this problem, the concentration of carbon was modified until no metallic iron remained in the composition. In the present work, two methodology of injection are compared to study their influence on the phase purity, size and morphology of the particles as well as their electrochemical properties. X-ray diffraction is used to verify the crystallinity and the purity of the phase obtained. The results show that a pure phase is obtained in optimized condition and samples with low amount of impurities like Fe2O3 are obianed when no optimization is done. The oxidation state of Fe in the samples, the nature of the impurities and the quantities are confirmed by Mossbauer spectroscopy. During calcination, we observed a phenomenon of carbothermal reduction which was evidenced by Mossbauer spectroscopy (Figure 1). SEM analysis shows the morphology of the obtained particles with a size range between 1,5𝜇m and 8𝜇m using bi-fluid and rotary nozzles, respectively. The electrochemical performances are tested by galvanostatic cycling in sodium half cells and show significant improvement with the optimization of morphology and carbon content. [less ▲]

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See detailOne Step Hydrothermal Synthesis of Fe1.19(PO4)(OH)0.57(H2O)0.43 composite cathode material and Its Electrochemical Properties in Li-Ion Batteries
Mahmoud, Abdelfattah ULiege; Karegeya, Claude; Sougrati, Moulay Tahar et al

Conference (2018, December 13)

Lithium-ion batteries (LIBs) have been widely applied as a power source for portable and stationary energy storage systems. In this work, we report the electrochemical performance of FPHH/CB and FPHH/CNT ... [more ▼]

Lithium-ion batteries (LIBs) have been widely applied as a power source for portable and stationary energy storage systems. In this work, we report the electrochemical performance of FPHH/CB and FPHH/CNT cathode materials for Li-ion batteries where FPHH represents Fe1.19(PO4)(OH)0.57(H2O)0.43 while carbon black (CB) and carbon nanotubes (CNT) were used as precursors in the one-pot hydrothermal synthesis. We show that the addition of conducting carbon black into the solution has a strong influence on reducing the particle size and tailoring their morphology. Thanks to its favorable microstructural characteristics, the FPHH-10 wt% C and FPHH-20 wt% C materials exhibited good performance [1]. The CNT also improve the performance of FPHH such as capacity retention. The study of the reaction mechanism of FPHH/CNT during cycling by combining operando XRD and 57Fe Mössbauer spectroscopy (Figure 1) shows that the insertion mechanism is a monophasic reaction with 10% volume variations associated to the Fe3+/Fe2+ redox reaction [2]. Acknowledgements A. Mahmoud is grateful to University of Liege and FRS-FNRS for the grants and thanks to the Walloon region for a Beware Fellowship Academia 2015-1, RESIBAT n° 1510399. Part of this work was supported by the Walloon Region under the “PE PlanMarshall2.vert” program (BATWAL – 1318146). References 1. C. Karegeya, A. Mahmoud, R. Cloots, B. Vertruyen, F. Boschini, Electrochimica Acta 250 (2017) 49-58. 2. A. Mahmoud, C. Karegeya, M. T. Sougrati, J. Bodart, B. Vertruyen, R. Cloots, P-E. Lippens, F. Boschini. ACS Applied Materials and interfaces 10 (2018) 34202-34211. [less ▲]

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See detailCrystal chemistry and polymorphism of an iron-tungsten mixed oxide
Caubergh, Stéphane ULiege; Jungers, Thomas ULiege; Mahmoud, Abdelfattah ULiege et al

Conference (2018, December 13)

Iron tungstate Fe2WO6 attracts increasing interest in two areas of applications due to its photoelectrochemical behaviour. Fe2WO6 is studied either as a photocatalyst for degradation of environmental ... [more ▼]

Iron tungstate Fe2WO6 attracts increasing interest in two areas of applications due to its photoelectrochemical behaviour. Fe2WO6 is studied either as a photocatalyst for degradation of environmental pollutants or as a photoanode for water oxidation in tandem devices. Recently, some of its magneto-dielectric properties have been reported but its magnetic and electric properties remain nebulous. Indeed, Fe2WO6 iron tungstate exists as two or three crystal structures with different organizations of the FeO6 and WO6 octahedra. The conditions of polymorphism are still unclear: structures were reported in the literature for only two of the three polymorphs (α and γ) and very little is known about the third polymorph (β). In the present work, we could synthesize for the first time a complete set of the three polymorphs as single-phase products by spray-drying, thereby confirming the existence of the β-polymorph. We revised the structural model for the α-polymorph and solved the structure of the β-polymorph. The new procedure of synthesis also allowed us to control and tune the Fe/W ratio and investigate the possibility for a solid solution domain. The final products were characterized by means of X-Ray Diffraction (synchrotron data), Rietveld refinement, Scanning Electron Microscopy and 57Fe Mossbauer spectroscopy. [less ▲]

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See detailSpray drying synthesis of Na3V2(PO4)2F3/C cathode material for Na-ion batteries: study of the effect of the carbon source on electrochemical performance
Eshraghi, Nicolas ULiege; Bodart, Jérôme ULiege; Mahmoud, Abdelfattah ULiege et al

Poster (2018, November 25)

Lithium-ion batteries have enjoyed great success and have outperformed other rechargeable battery system since 1980. However, Li-ion batteries face many challenges and limitations: safety, the low ... [more ▼]

Lithium-ion batteries have enjoyed great success and have outperformed other rechargeable battery system since 1980. However, Li-ion batteries face many challenges and limitations: safety, the low abundance of lithium in the Earth’s crust. Recently, Sodium-ion batteries attracted a lot of interest as a potential alternative to lithium-ion batteries for large-scale energy storage applications, due to the large natural abundance and lower cost of sodium. In recent years, fluorophosphates with the NASICON (Na Super-Ionic Conductor) type structure are considered among the most interesting series of cathode materials for Li/Na-ion batteries, because they exhibit rich chemistry, attractive lithium/sodium insertion properties and thus offer promising electrochemical properties [1]. Na3V2(PO4)2F3 (NVPF) attracted high attention thanks to its promising electrochemical properties. The inductive effects of both PO43- and F- allow for a high working potential combined with a high theoretical specific capacity due to the multiple oxidation states of vanadium[1-2]. One of the key drawbacks of Na3V2(PO4)2F3 electrodes is their low intrinsic electronic conductivity. NVPF and NVPF/carbon composite materials were prepared by spray-drying method using the same conditions used in our previous work [2]. Spray drying is a cost-effective and easily up-scalable route to prepare homogeneous multi-component powders, thus making it a suitable method to incorporate carbon in the composite powder. We used different carbon sources like conductive carbons (MWCNTs, Carbon Black, etc) and organic sources (PVA, Citric Acid, Ascorbic acid, etc) to prepare NVPF/carbon composite powders. the structural, electrochemical, and morphological properties of the synthesized Na3V2(PO4)2F3/C samples were systematically investigated in order to understand the influence of carbon source on structural and morphological properties and most importantly electrochemical performance of NVPF and NVPF/carbon composite cathode materials for Na-ion batteries. The chemical diffusion of Na ions was studied using results obtained by varying scan rates in cyclic voltammetry measurements. Raman spectroscopy is used to evaluate the quality in disordered carbon materials and its electronic conductivity [3] and compared the results with the results from EIS and cycling performance of different samples. Acknowledgments The authors are grateful to University of Liege and FRS-FNRS for grants. Part of this work was supported by the Walloon Region under the “PE PlanMarshall2.vert” program (BATWAL – 1318146). A. Mahmoud thanks to the Walloon region for a Beware Fellowship Academia 2015-1, RESIBAT n° 1510399. References: [1] R. A. Shakoor, D-H. Seo, H. Kim, Y-U. Park, J. Kim, S-W. Kim, H. Gwon, S. Leec and K. Kang, Mater. Chem. 22 (2012) 20535–20541. [2] N. Eshraghi, S. Caes, A. Mahmoud, R. Cloots, B. Vertruyen, F. Boschin, Electrochimica Acta, 228, (2017), 319-324. [3] A. Mahmoud, S. Caes, M. Brisbois, R. P. Hermann, L. Berardo, A. Schrijnemakers, C. Malherbe, G. Eppe, R. Cloots, B. Vertruyen, F. Boschin J Solid State Electrochem. 22 (2018) 103-112. [less ▲]

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See detailElectrochemical mechanism and effect of carbon addition during hydrothermal synthesis to improve the electrochemical performance of Fe1.19(PO4)(OH)0.57(H2O)0.43 cathode material for Li-ion batteries
Mahmoud, Abdelfattah ULiege; karegeya, Claude; Sougrati, Moulay Tahar et al

Poster (2018, November 25)

Since the introduction of lithium-ion batteries (LIBs) to market in 1991, their performance has improved significantly, which has been achievable through development in materials technologies. However ... [more ▼]

Since the introduction of lithium-ion batteries (LIBs) to market in 1991, their performance has improved significantly, which has been achievable through development in materials technologies. However, further breakthroughs are still needed to ameliorate cycle-life, safety and energy density of LIBs. This requires new electrode materials and a detailed understanding of the electrochemical mechanisms during cycling. Transition metal phosphates are interesting candidates as cathode materials for LIBs [1]. In this work, we report the electrochemical performance of FPHH/C and FPHH/CNT composites where FPHH represents Fe1.19(PO4)(OH)0.57(H2O)0.43 while carbon black and carbon nanotubes (CNT) were used as precursors in the one-pot hydrothermal synthesis, respectively. We show that the addition of conducting carbon black into the solution has a strong influence on reducing the particle size and tailoring their morphology, but does not interfere with the formation of the FPHH phase. Thanks to its favorable microstructural characteristics, the FPHH-10 wt% C and FPHH-20 wt% C materials exhibited good performance [2]. The CNT also improve the performance of FPHH such as capacity retention (500 cycles at 1 C). The mechanisms of lithiation-delithiation were investigated by combining operando X-ray diffraction and 57Fe Mössbauer spectroscopy. FPHH undergoes a monophasic reaction based on Fe3+/Fe2+ redox process. However, the variations of the lattice parameters and 57Fe quadrupole splitting indicate a more complex mechanism than a random occupation of the vacant sites within FPHH. This can be related to the peculiar structure of FPHH formed by chains of face sharing (Fe0.6•0.4)O6 octahedra connected by PO4 tetrahedra and by channels for Li diffusion along [100] and [010] directions. The existence of Fe vacancies provide interconnections between the one-dimensional channels, improving lithium diffusion within FPHH. This mechanism, combined with the addition carbon black or nanotubes in the solution prior to hydrothermal treatment as a simple and effective way to reduce particle size and improve electronic conductivity, provides good cycle life and rate capability for FPHH. Acknowledgements A. Mahmoud is grateful to University of Liege and FRS-FNRS for the grants and thanks to the Walloon region for a Beware Fellowship Academia 2015-1, RESIBAT n° 1510399. Part of this work was supported by the Walloon Region under the “PE PlanMarshall2.vert” program (BATWAL – 1318146). References 1. C. Karegeya, A. Mahmoud, F. Hatert, B. Vertruyen, R. Cloots, P.E. Lippens, F. Boschini, Journal of Power Sources 388 (2018) 57-64. 2. C. Karegeya, A. Mahmoud, R. Cloots, B. Vertruyen, F. Boschini, Electrochim. Acta 250 (2017) 49-58. [less ▲]

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