Publications of Rudi Cloots
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See detailFlexible thin-films for battery electrodes
Piffet, Caroline ULiege; Boschini, Frédéric ULiege; Cloots, Rudi ULiege

Patent (2018)

A composition comprising: a. An at least partially hydrolysed polyvinyl acetate component having an hydrolysation degree of at least 5%, b. A polyalkylene glycol component having a number average ... [more ▼]

A composition comprising: a. An at least partially hydrolysed polyvinyl acetate component having an hydrolysation degree of at least 5%, b. A polyalkylene glycol component having a number average molecular mass Mn lower than 9000 g/mol and consisting of one or more substances selected from the group consisting of polyethylene glycol, polypropylene glycol, copolymers of ethylene glycol and propylene glycol, and their derivatives, c. a positive or negative electrode active component, and d. a conductive component, wherein the mass ratio between the at least partially hydrolysed polyvinyl acetate component and the positive or negative electrode active component equals at least 0.12 and at most 0.30, and wherein the mass ratio between the polyalkylene glycol component and the positive or negative electrode active component equals at least 0.012 and at most 0.10 [less ▲]

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See detailHeterostructured ZnO/RuO2 photocatalyst: influence of sputtering temperature on the photocatalytic and photoelectrochemical properties
Periyannan, Shanmugapriya ULiege; Manceriu, Laura ULiege; Colson, Pierre ULiege et al

Poster (2018, June 19)

Influence of thermal conditions on the performance of heterostructured ZnO/RuO2 in their photocatalytic and photoelectrochemical properties Photocatalytic materials are highly investigated due its vital ... [more ▼]

Influence of thermal conditions on the performance of heterostructured ZnO/RuO2 in their photocatalytic and photoelectrochemical properties Photocatalytic materials are highly investigated due its vital role in wide variety of applications that could help in tackling present day environmental problems. Inspite of wide and basic investigation for several decades on promising materials, the best photocatalyst is still under research. But the decades long research helped in better understanding of the materials and mechanisms involved. This led to the improvement of materials under examination from homostructured to modified materials. One of the major limiting factors of homostructured (single) photocatalyst is the fast recombination of excited charge carriers. Among several modification techniques used to enhance the lifetime of charge carriers, heterostructure formation with two different materials is very promising. Here, we report the formation of ZnO/RuO2 by involving two steps: ZnO nanorods are grown on FTO by hydrothermal method, followed by physical deposition of RuO2 (At room temperature [RT], At RT followed by Insitu-Post Annealing at 250° & At High Temperature [HT] 400°), resulting in the formation of a heterostructure. The influence of different thermal conditions on the course of RuO2 deposition has been characterized by X-Ray Diffractometer (XRD), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), X-Ray Photoelectron Spectroscopy (XPS) and Photo Luminescence (PL). The crystallinity of the material and its orientation was examined by XRD. Morphological studies by SEM revealed the growth of randomly oriented ZnO nanorods on FTO, whereas images of ZnO/RuO2 resulted in no structural difference. A very thin layer of RuO2 covering the surface of ZnO nanorods was observed through TEM. This displayed the core-shell type of heterostructure formation. XPS studies of ZnO/RuO2 under varying conditions implied the shift towards lower binding energy, which indicates the bond sharing between both materials. Interface studies by step-wise deposition of RuO2 on ZnO, showed the evidence for formation of band bending between two materials, which play an important role in enhancing the charge carrier separation. PL of homostructured and heterostructured materials led to the understanding with carrier recombination process. There was evidence of significant quenching for ZnO/RuO2, compared to that of ZnO. Among ZnO/RuO2 (At RT, RT-PAd, HT) – deposition at 400° disclosed higher quenching, i.e., reduced rate of recombination. Photocatalytic and Photoelectrochemical investigations was clearly correlating to the characterizational studies, confirming the enhancement in performance with heterostructure, especially with the ZnO/RuO2 (400°). [less ▲]

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See detailInsight into the electrical properties damaging with quenching of the SnO2:F layers
Manceriu, Laura ULiege; Maho, Anthony ULiege; Labrugère, Christine et al

Conference (2018, June 18)

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See detailNa1.25Ni1.25Fe1.75(PO4)3 nanoparticles as a janus electrode material for Li-ion batteries
Karegeya, Claude; Mahmoud, Abdelfattah ULiege; Hatert, Frédéric ULiege et al

in Journal of Power Sources (2018), 388

Abstract A solvothermal method was used to prepare Na1.25Ni1.25Fe1.75(PO4)3 nanoparticles, a new promising electrode material for lithium-ion batteries. The composition and the crystal structure were ... [more ▼]

Abstract A solvothermal method was used to prepare Na1.25Ni1.25Fe1.75(PO4)3 nanoparticles, a new promising electrode material for lithium-ion batteries. The composition and the crystal structure were determined by 57Fe Mössbauer spectroscopy and powder X-ray diffraction Rietveld refinements and confirmed by magnetic measurements. The structural formula □0.75Na1.25Ni1.25Fe1.75(PO4)3 was obtained showing a significant amount of Na vacancies, which enhances Li diffusion. Na1.25Ni1.25Fe1.75(PO4)3 was used as negative and positive electrode material and shows excellent electrochemical performances. As negative electrode in the voltage range 0.03-3.5 V vs. Li+/Li, the first discharge at current density of 40 mA g−1 delivers a specific capacity of 1186 mAh g−1, which is almost three times its theoretical capacity (428 mAh g−1). Then, reversible capacity of 550 mAh g−1 was obtained at 50 mA g−1 with high rate capability (150 mAh g−1 at 500 mA g−1) and capacity retention of 350 cycles. As positive electrode material, specific capacities of about 145 and 99 mAh g−1 were delivered at current densities of 5 and 50 mA g−1, respectively, in the voltage range of 1.5–4.5 V vs. Li+/Li. In addition, we show that the use of solvothermal synthesis contributes to the synthesis of small sized particles leading to good electrochemical performances. [less ▲]

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See detailComposites Fe1.19(PO4)(OH)0.57(H2O)0.43/C comme matériaux d'électrode positive pour batteries Li-ion
Mahmoud, Abdelfattah ULiege; karegeya, Claude; Sougrati, Moulay Tahar et al

Conference (2018, May 17)

Les matériaux composites Fe1.19(PO4)(OH)0.57(H2O)0.43-C (FPHH-C) ont été obtenus par synthèse hydrothermale en une seule étape. L'addition du noir de carbone dans la solution contenant les précurseurs ... [more ▼]

Les matériaux composites Fe1.19(PO4)(OH)0.57(H2O)0.43-C (FPHH-C) ont été obtenus par synthèse hydrothermale en une seule étape. L'addition du noir de carbone dans la solution contenant les précurseurs avant la réaction hydrothermale (2, 10 et 20 %m) a conduit à une réduction de la taille des particules de FPHH avec une bonne dispersion du carbone conducteur électronique autour et entre les particules. La caractérisation des composites par diffraction des rayons X et spectroscopie Mössbauer du 57Fe montre que l'ajout de carbone ne modifie pas la pureté des matériaux mais améliore significativement les propriétés électrochimiques pour FPHH - 10 %m et FPHH - 20 %m par rapport à FPHH et FPHH - 2 %m [1]. Une étude du mécanisme d'intercalation et de désintercalation du lithium a été effectuée en associant diffraction des rayons X et spectroscopie Mössbauer operando [2]. L’analyse de l’ensemble des résultats montre que ce mécanisme est une réaction d'intercalation monophasique réversible associée au couple redox Fe3+/Fe2+. L’excellente réversibilité observée sur plus de 500 cycles avec des variations volumiques de 10% confirme la bonne stabilité de ce matériau. Remerciements Ab. Mahmoud remercie la région wallonne pour le projet RESIBAT n°1510399. Références 1. C. Karegeya, A. Mahmoud, R. Cloots, B. Vertruyen, F. Boschini, Electrochim. Acta 250 (2017) 49-58. 2. K. Lasri, A. Mahmoud, I. Saadoune, M-T. Sougrati, L. Stievan, P-E. Lippens, R. P. Hermann, H. Ehrenberg, Sol. Energ. Mater. & Sol. Cells148 (2016) 11–19. [less ▲]

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See detailLa souris, le patient, et le faux expert. Décryptage d'une mystification.
Bakker, Julie ULiege; Balthazart, Jacques ULiege; Baron, Frédéric ULiege et al

Article for general public (2018)

La recherche sur animaux est actuellement encadrée de façon stricte en Wallonie comme dans toute l'Union Européenne (voir l'article de Marc Vandenheede publié dans le Vif). Cette législation et les ... [more ▼]

La recherche sur animaux est actuellement encadrée de façon stricte en Wallonie comme dans toute l'Union Européenne (voir l'article de Marc Vandenheede publié dans le Vif). Cette législation et les contrôles qui y sont associés induisent de nombreuses contraintes pratiques, des charges administratives et des coûts financiers importants que les chercheurs seraient certainement heureux d'éviter s'il existait une alternative à l'expérimentation animale. [less ▲]

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See detailAnalyse détaillée de la seconde version de l’avant-projet de Code du bien-être animal wallon. Lecture commentée au 21/03/2018 du Chapitre 8 (Expérimentation animale)
Drion, Pierre ULiege; Corhay, Albert ULiege; Haubruge, Eric ULiege et al

Report (2018)

La compétence « bien-être animal », auparavant fédérale, a été régionalisée en juillet 2014. Ce projet de code vise à remplacer les dispositions légales en vigueur (la Loi de 1984 telle que modifiée par ... [more ▼]

La compétence « bien-être animal », auparavant fédérale, a été régionalisée en juillet 2014. Ce projet de code vise à remplacer les dispositions légales en vigueur (la Loi de 1984 telle que modifiée par les décrets du Gouvernement wallon). Certains éléments sont repris tels quels de la Directive 2010/63. Cela est nécessaire car la Directive européenne en tant que telle n’a pas de force obligatoire en Belgique. Elle doit être transcrite par un instrument législatif (avant, la Loi de 1984 et ses modifications, aujourd’hui, le projet de code pour la Région wallonne). Certains aspects semblent flous, mais renvoient à des dispositions que le Gouvernement doit encore prendre (au travers d’arrêtés du Gouvernement wallon, comme le faisaient avant les nombreux arrêtés royaux et du gouvernement qui réglementent la matière). Les arrêtés d’exécution devront obligatoirement tenir compte de la Directive européenne et s’inspirer de dispositions actuellement en vigueur. [less ▲]

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See detailOpal-like photoanodes with photonic effects in macroporous perovskite solar cells
Dewalque, Jennifer ULiege; Baron, Damien ULiege; Spronck, Gilles ULiege et al

Poster (2018, February 28)

Organic-inorganic metal halide perovskite compounds, used either in mesoscopic or planar solar cells architectures, have allowed preparing highly efficient solid-state devices (>20%). In mesoscopic solar ... [more ▼]

Organic-inorganic metal halide perovskite compounds, used either in mesoscopic or planar solar cells architectures, have allowed preparing highly efficient solid-state devices (>20%). In mesoscopic solar cells, a mesoporous TiO2 scaffold is incorporated into the cells. However, because of the small pore size compared to the wavelengths of visible light, the scaffold barely scatters light. In this work, we propose to design periodically structured TiO2 scaffold from colloidal crystal templating fabrication method. Polystyrene beads with diameters comparable to visible light wavelengths are used as structuring agent. The resulting opal-like photonic structure will strongly interact with light and increase light harvesting. The photoanode microstructure is characterized by scanning electron microscopy (SEM) and X-Ray diffraction (XRD). In parallel, light interaction is modeled in order to find the best compromise in terms of photonic architecture. Sunlight absorption by the solar cells is presented and discussed with dependency of pore sizes and number of opal-like layers. [less ▲]

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See detailPreparation of p-type Bi2Sr2Co2Ox and n-type doped CaMnO3 polycrystalline thermoelectric bulk materials by Pilot Spray Drying processing way
Combe, Emmanuel ULiege; Bastin, Frédérique; Caes, Sébastin et al

Conference (2017, December 13)

Since decades, thermoelectricity is deeply studied as no-waste energy source. Thermoelectric (TE) materials allow the direct transformation of a heat source into an electrical current (Seebeck effect). TE ... [more ▼]

Since decades, thermoelectricity is deeply studied as no-waste energy source. Thermoelectric (TE) materials allow the direct transformation of a heat source into an electrical current (Seebeck effect). TE conversion is very attractive as it is the strongest candidate for producing electricity from waste heat energy sources (automobiles, incinerators, boilers, …). For TE applications at high temperatures, oxide compounds have attracted attention, in particular due to their natural oxidation resistance. However, for large scale utilization of TE conversion systems, performances of actual TE oxides compounds must be improved. Among the different studied oxide compositions, misfit cobaltite Bi2Sr2Co2Ox and doped calcium manganate CaMnO3- have attracted much attention, as p and n-type oxide TE elements, respectively. Bi2Sr2Co2Ox (abbreviated BSC-222) material exhibits a layered structure, composed of CoO2 layers which alternate with Bi2Sr2O4 block layers along the c-axis. Such crystallographic structure allows interesting electrical and thermal properties, suitable for reaching high TE performances. On the other hand, CaMnO3- compound (abbreviated as CMO) has an orthorhombic perovskite-type structure with interesting TE properties. Reaching high TE performances requires using new processing way. Indeed, conventional solid-state reaction does not allow controlling the microstructure of materials, i.e. the shape, size, or alignment of grains, size and distribution of porosity of samples. Those parameters play a major role on the electrical and thermal transport properties. With the aim of developing a processing method which can be easily transposable to an industrial level in terms of simplicity, speed, large-scale production and cost, a pilot spray-drying processing method has been developed for the production of BSC-222 and CMO thermoelectric powders. Spray-drying is a processing way in which preparing powders is achieved by passing a solution, or a suspension, in a stream of hot air. By using solutions, or suspensions, of precursor compounds, a more homogeneous dispersion of the cations into the material is reaching. Spray-dried powders are so more reactive, which can help reducing the sintering temperature or duration. This study deals with the preparation of BSC-222 and doped CMO thermoelectric powders by the development of spray-drying method. Contrary to CMO powders, prepared from solution of cations, BSC-222 powders have been prepared from Bi2O3-Co3O4-SrCO3 suspensions. For that purpose, a preliminary study of the stability of the precursors in the suspension’s solvent has been conducted in order to favor a homogeneous distribution of precursors in prepared spray-dried powders. After calcination thermal treatment, spray dried powders with BSC-222 or CMO compositions have been successfully obtained. Polycrystalline BSC-222 and CMO bulk materials have been then prepared by conventional sintering. In this study, we report also on the thermoelectric properties, carried out up to 1000 K, of such prepared polycrystalline bulk materials and compare these with those reported in literature. [less ▲]

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See detailHydrothermal self-assembly of sodium manganese iron phosphate particles: Growth mechanism and electrochemical performance in lithium-ion battery
Karegeya, claude; Mahmoud, Abdelfattah ULiege; Vertruyen, Bénédicte ULiege et al

in Solid State Ionics (2017), 312

Na2Mn1.5Fe1.5(PO4)3 (NMFP) dandelion sphere-like particles were successfully synthesized via a hydrothermal route without addition of any templates or surfactants (laboratory and pilot scales). The ... [more ▼]

Na2Mn1.5Fe1.5(PO4)3 (NMFP) dandelion sphere-like particles were successfully synthesized via a hydrothermal route without addition of any templates or surfactants (laboratory and pilot scales). The hydrothermal reactor (pilot scale) is equipped with stirrer for continuous agitation of reagents during the reaction. The obtained materials were characterized by X-ray diffraction, Mössbauer spectroscopy and Scanning electron microscopy. Results show that Na2Mn1.5Fe1.5(PO4)3 samples obtained from the reaction performed at laboratory scale have hierarchical dandelion sphere-like morphology and the dandelions consist of micro-/nano-rods. On the other hand, we obtained the self-assembly nano-rods morphology for the particles prepared using hydrothermal reactor. On the basis of the experimental results, a growth mechanism of Na2Mn1.5Fe1.5(PO4)3 self-assembly and dandelion sphere-like particles was proposed. Temperature and time of hydrothermal reaction are found to be crucial parameters in controlling the growth of Na2Mn1.5Fe1.5(PO4)3 particles. In addition, investigation of the effect of continuous stirring during the hydrothermal reaction shows that the reaction time can be optimized to obtain Na2Mn1.5Fe1.5(PO4)3 with small particles size. The influence of stirring on the NMFP morphology has been clearly evidenced. Indeed, the stirring leads to homogeneous particles. Cycling studies have shown that the synthesized Na2Mn1.5Fe1.5(PO4)3 dandelions materials exhibit specific discharge capacities of about 62 and 57 mAh g−1 equivalent to about 1.2 and 1.05 lithium ions de-intercalated at C/15 and C/10 current density respectively. [less ▲]

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See detailElectrode materials for Li/Na-ion batteries: Improving electrochemical performance through carbon addition during synthesis
Mahmoud, Abdelfattah ULiege; Karegeya, Claude; Eshraghi, Nicolas ULiege et al

Poster (2017, October 12)

Lithium-ion batteries have been widely applied as a power source for portable and stationary energy storage systems. Na-ion batteries are considered to be an alternative to Li-ion batteries owing to the ... [more ▼]

Lithium-ion batteries have been widely applied as a power source for portable and stationary energy storage systems. Na-ion batteries are considered to be an alternative to Li-ion batteries owing to the natural abundance of sodium. New electrode materials are required to increase the energy density of Li/Na-ion batteries. In this study, we show that the addition of the carbon sources during the synthesis leads to control the particles size and morphology and improve their conductivity properties that enhance the electrochemical performance [1-5]. In order to study the effect of the carbon on the structural, morphological and electrochemical properties of the prepared materials by a spray-drying [1-3] or hydrothermal methods [4, 5]. The crystal and local structure were analyzed by XRD and Mössbauer spectroscopy. The morphological properties were characterized by SEM and TEM. The carbon content was determined by TG/TDA and carbon analyzer. The electrochemical properties were studied by impedance spectroscopy and galvanostatic cycling in lithium cells. Finally, the reaction mechanism during cycling was investigated using operando XRD technique. 1- A. Mahmoud, S. Caes, M. Brisbois, R.P. Hermann, L. Berardo, A. Schrijnemakers, C. Malherbe, G. Eppe, R. Cloots, B. Vertruyen, F. Boschini, Spray-drying as a tool to disperse conductive carbon inside Na2FePO4F particles by addition of carbon black or carbon nanotubes to the precursor solution, J. Solid State Electrochem. (2017) 1–10. 2- N. Eshraghi, S. Caes, A. Mahmoud, R. Cloots, B. Vertruyen, F. Boschini, Sodium vanadium (III) fluorophosphate/carbon nanotubes composite (NVPF/CNT) prepared by spray-drying: good electrochemical performance thanks to well-dispersed CNT network within NVPF particles, Electrochim. Acta, 228 (2017) 319–324. 3- M. Brisbois, S. Caes, M-T. Sougrati, B. Vertruyen, A. Schrijnemakers, R. Cloots, N. Eshraghi, R-P. Hermann, A. Mahmoud, F. Boschini, Na2FePO4 F/multi-walled carbon nanotubes for lithium-ion batteries: Operando Mössbauer study of spray-dried composites, Solar Energy Materials & Solar Cells 148 (2016) 67-72. 4- C. Karegeya, A. Mahmoud, B. Vertruyen, F. Hatert, R.P. Hermann, R. Cloots, F. Boschini, One-step hydrothermal synthesis and electrochemical performance of sodium-manganese-iron phosphate as cathode material for Li-ion batteries, J. Solid State Chem.253 (2017) 389–397. 5- C. Karegeya, A. Mahmoud, R. Cloots, B. Vertruyen, F. Boschini, Hydrothermal synthesis in presence of carbon black: Particle-size reduction of iron hydroxyl phosphate hydrate for Li-ion battery, Electrochimica Acta. Electrochim. Acta 250 (2017) 49–58. [less ▲]

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See detailA SPRAY DRYING METHOD FOR THE PREPARATION OF Na2FePO4F/CB AND Na2FePO4F/CNT COMPOSITES CATHODE FOR LITHIUM-ION BATTERIES
Mahmoud, Abdelfattah ULiege; Berardo, Loris ULiege; Brisbois, Magali et al

Poster (2017, September 18)

Fluorophosphates are considered among the most interesting series of cathode material for Li/Na-ion batteries1. Na2FePO4F (space group Pbcn), with its layered structure and two-dimensional pathways for ... [more ▼]

Fluorophosphates are considered among the most interesting series of cathode material for Li/Na-ion batteries1. Na2FePO4F (space group Pbcn), with its layered structure and two-dimensional pathways for facile Na+/Li+ transport, exhibits minimal structural changes upon reduction/oxidation. The average working voltage is 3.3 V vs. Li/Li+. Intercalation/deintercalation results in a volume change of only 3.7%. However, one of the key drawbacks of Na2FePO4F electrodes is their low intrinsic electronic conductivity. In order to study the effect of the carbon black and carbon nanotubes on the electrochemical performance of Na2FePO4F cathode material for lithium-ion batteries, Na2FePO4F, Na2FePO4F/CB and Na2FePO4F/CNT were prepared by a spray-drying method with different ratios of CB and CNT (10 and 20%). The crystal and local structure were analyzed by XRD and Mössbauer spectroscopy. The electrochemical properties were studied by galvanostatic cycling in lithium cells. The electrochemical performance is markedly better in the case of Na2FePO4F/CNT (20 wt%), with specific capacities of about 100 mAh/g (Na2FePO4F/CNT) at C/4 rate2 vs. 50 mAh/g for Na2FePO4F/CB. The characterization of Na2FePO4F/CB particles by electron microscopy revealed a carbon-poor surface and a good carbon dispersion for Na2FePO4F/CNT particles attributed to better diffusion of carbon nanotubes in the droplets during drying. References : 1-N. Eshraghi, S. Caes, A. Mahmoud, R. Cloots, B. Vertruyen, F. Boschini, Electrochim. Acta, 228 (2017) 319–324. 2-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) 67-72. [less ▲]

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See detailComparison of the electrochemical performance of Li4Ti5O12 spinel as negative electrodes for lithium-ion batteries prepared by sol gel and spray drying methods
Mahmoud, Abdelfattah ULiege; Piffet, Caroline ULiege; Berardo, Loris ULiege et al

Poster (2017, September 05)

Energy is considered as the lifeblood of modern society. Rechargeable batteries are the most promising to meet the human needs concerning the energy storage thanks their high energy density and high ... [more ▼]

Energy is considered as the lifeblood of modern society. Rechargeable batteries are the most promising to meet the human needs concerning the energy storage thanks their high energy density and high energy efficiency. Most difficult challenges of the development of promising rechargeable batteries concern the electrode materials. Li4Ti5O12 (LTO) is one the most promising anode materials for Li-ion batteries, as it demonstrates very stable cycling stability and excellent safety. Its high operating potential (~1.5 V) allows to avoid the formation of SEI during the first cycle. The three-dimensional structure offers LTO excellent reversibility due to the near zero volume strain during the Li+ ion intercalation and deintercalation cycling. The main objective of this study on LTO samples was to evidence the effect of synthesis method and thermal conditions on their structural, morphological and electrochemical properties [1, 2]. The results demonstrate the strong influence of the synthesis route (Sol-Gel and spray-drying methods) and the thermal treatment on the capacity, cyclability and rate capability of the LTO spinel in Li-half-cell and Li-ion full-cell (see Figure 1). References [1] A. Mahmoud, J. M. Amarilla, K. Lasri, I. Saadoune, Electrochim. Acta 93 (2013) 163-172. [2] A. Mahmoud, J. M. Amarilla, I. Saadoune, Electrochim. Acta 163 (2015) 213-222. [less ▲]

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See detailUp-scalable spray-drying synthesis of Na2Ti3O7
Piffet, Caroline ULiege; Vertruyen, Bénédicte ULiege; Mahmoud, Abdelfattah ULiege et al

Poster (2017, September)

Detailed reference viewed: 58 (9 ULiège)