
Damien SaurelCIC Energigune · Electrochemical Energy Storage (EES)
Damien Saurel
PhD
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Publications (76)
Manganese (Mn) substitution is a widely explored strategy aimed at sustainably enhancing the energy density of iron (Fe)-based electrode materials by taking advantage of the higher redox potential of the former. However, excessive Mn content can lead to detrimental effects, offsetting the expected improvements. In experimental studies, triphylite N...
The translation of inorganic–polymer hybrid battery materials from laboratory-scale to industry-relevant battery manufacturing processes is difficult due to their complexity, scalability, and cost and the limited fundamental knowledge that is available. Herein, we introduce a unique and compelling approach for the preparation of hybrid solid electr...
Blended positive electrodes consisting of mixtures of LiMn2O4 spinel (LMO) and layered LiNi0.5Mn0.3Co0.2O2 (NMC) have been studied by coupling electrochemical testing to operando synchrotron based X-ray absorption and powder diffraction experiments to shed light on their redox mechanism. Blending NMC with LMO results in enhanced energy density at h...
Transition metal (TM) layered oxides constitute a promising family of materials for use in Na-ion battery cathodes. Here O3-Na (Ni1/3Mn1/3Fe1/3) O2 was synthesised using optimised sol-gel and solid-state routes, and the physico- and electrochemical natures of the resulting materials were thoroughly studied. Significant differences in electrochemica...
By applying solid-state 6,7 Li NMR, we reveal a redox reaction sequence of solid solution and biphasic transition and highlight the existence of intermediate species in non-stoichiometric transition metal-ordered high-voltage LNMO cathode reaction vs. Li.
Mn-substitution in triphylite NaFe1-yMnyPO4 is here explored with the aim to enhance the electrochemical performance of NaFePO4. Our results show that, similarly to the LiFe1-yMnyPO4 system, increasing the Mn-content raises the average discharge voltage but this comes at the expense of limiting the capacity. However, y = 0.2 is identified as an opt...
Graphite ineffectiveness in sodium storage has induced extensive research on non-graphitic carbons as high-performance active materials for negative electrodes of Na-ion batteries. Among these, soft carbons are promising for high-power sodium storage, yet their practical success is jeopardized by their low initial coulombic efficiency (i.e. 65-70%)...
Battery electrodes materials undergo significant mechanical instabilities which affect their longevity and exert rate-limitations during the cycling process. In this study, we investigate the rate-dependent mechanical response of sodium iron phosphate (NaFePO4, NFP) cathodes during Na intercalation via galvanostatic cycling at different rates by em...
Invited for this month's cover is the group of Damien Saurel and Montserrat Canas‐Cabanas at CIC EnergiGUNE and Ikerbasque (Spain). the data corresponding to NaTiOPO4 Na‐ion anode material obtained in a powder X‐ray diffraction operando experiment when cycled between 2.4 and 1V vs Na+/Na (2θ λ Cu = 32° ‐ 34 °, reversible intercalation of 0.58 Na+)....
The Front Cover shows the data corresponding to NaTiOPO4 Na‐ion anode material obtained in a powder X‐ray diffraction operando experiment when cycled between 2.4 and 1V vs Na+/Na (2θ λ Cu = 32° ‐ 34 °, reversible intercalation of 0.58 Na+). Operando experiments have provided key insights regarding the internal processes occurring in a battery durin...
Operando experiments represent a powerful tool for the monitoring of internal processes upon battery cycling that provide valuable insights regarding the fundamental electrochemical redox mechanisms and ageing phenomena in battery materials. However, obtaining high‐quality, representative and exploitable data from operando measurements requires car...
Hard carbon (HC) is the negative electrode (anode) material of choice for sodium‐ion batteries (SIBs). Despite its advantages in terms of cost and sustainability, a comprehensive understanding of its microstructure is not complete yet, thus hindering a rational design of high‐performance HC electrodes. In this study, rather than investigating how t...
Several emerging battery technologies are currently on endeavour to take a share of the dominant position taken by Li-ion batteries in the field of energy storage. Among them, sodium-based batteries offer a combination of attractive properties i.e., low cost, sustainable precursors and secure raw material supplies. Na-based batteries include relate...
Transition metal layered oxides (TMLOs) of general formula LiTMO 2 are the cornerstone of the present Li-ion technology as these cathode active materials allow the highest energy density thanks to the large capacity they offer. This is due to the high concentration of alkali metal their structure includes in the form of Li layers between TMO 2 meta...
Solid-state batteries with a Li metal anode and polymer–ceramic electrolytes hold the promise to boost safety and energy density, provided that stable conductive interfaces are achieved. Here, by focusing on the composite electrolyte system LLZO–PEO(LiTFSI), i.e., Li-ion conductive doped-Li7La3Zr2O12 (LLZO) garnet fillers embedded within the Li-ion...
The viability of the sodium-ion batteries as a post-lithium storage technology is strongly tied to the development of high-performance carbonaceous anode materials. This requires screening novel precursors, and tuning their electrochemical properties. Soft carbons as promising anode materials, not only for batteries, but also in hybrid capacitors,...
Ordered and disordered carbonaceous materials cover a wide range of the energy storage materials market. In this work a thorough analysis of the Small Angle X-ray Scattering (SAXS)patterns of a number of carbon samples for energy storage (including graphite, soft carbon, hard carbon, activated carbon, glassy carbon and carbide-derived carbon)is sho...
P2-type Na2/3Mn0.8Fe0.1Ti0.1O2, a promising high-performance electrode material for use in ambient temperature sodium-ion batteries, is examined using operando and long-term in situ synchrotron X-ray diffraction studies to reveal the structural evolution during battery function. Variable current cycling at current rates as high as 526 mA g−1 (4C) o...
The effect of water on the properties of superconcentrated sodium salt solutions in ionic liquids (ILs) was investigated to design electrolytes for sodium battery applications with water as an additive. Water was added to a 50 mol % solution of NaFSI [FSI=bis(fluorosulfonyl)imide] in the ionic liquid N‐methyl‐N‐propylpyrrolidinium bis(fluorosulfony...
Hard carbons are extensively studied for application as anode materials in sodium-ion batteries, but only recently a great interest has been focused toward the understanding of the sodium storage mechanism and the comprehension of the structure–function correlation. Although several interesting mechanisms have been proposed, a general mechanism exp...
Highly concentrated solutions of sodium bis(fluorosulfonyl)imide (NaFSI) with a series of bis(fluorosulfonyl)imide-based ionic liquids incorporating either alkyl phosphonium or alkoxy ammonium cations (P111i4FSI:NaFSI, P1i4i4i4FSI:NaFSI), N2(2O2O1)3FSI:NaFSI) are combined with NaFePO4 cathodes to demonstrate excellent cycling performance with respe...
Transition metal (TM) layered oxides constitute one of the most promising family of compounds for the cathode of Na-ion batteries. However, their structural stability at charged state is a critical performance limiting factor, which is believed to be closely related with irreversible TM migration into the Na layers. Nevertheless, experimental evide...
The investigation of phosphoric acid treatment on the performance of hard carbon from a typical lignocellulosic biomass‐waste (peanut shell) is herein reported. A strong correlation is discovered between the treatment time and the structural properties and electrochemical performance in sodium‐ion batteries. Indeed, a prolonged acid treatment enabl...
When electrode materials are driven away from equilibrium conditions, significant differences occur in their (dis)charge mechanism. In this paper, the changes in the phase transformations of the olivine NaFePO4 are examined as a function of the cycling rate from the thorough analyses of both the voltage‐composition profiles of galvanostatic cycling...
While sodium-ion batteries (SIBs) represent a low-cost substitute for Li-ion batteries (LIBs), there are still several key issues that need to be addressed before SIBs become market-ready. Among these, one of the most challenging is the negligible sodium uptake into graphite, which is the keystone of the present LIB technology. Although hard carbon...
Abstract We report a systematic study of the structural and magnetic properties of frustrated compounds of GaxMn(3−x)O4 (1.2 ≤ x ≤ 1.6) prepared by solid-state reaction. Using Rietveld refinement of X-ray diffraction patterns and O'Neill-Navrotsky model, we demonstrate that the system GaxMn(3−x)O4 (1.2 ≤ x ≤ 1.6) is an inverse spinel with low inver...
There is growing interest in ionic liquid based electrolytes for Na metal and Na-ion batteries. Here we compare three quite distinct bis(fluorosulfonyl)imide (FSI) anion based ionic liquids with small alkyl phosphonium (trimethyl isobutyl phosphonium, methyl tri-isobutyl: P111i4, P1i4i4i4) or alkoxy ammonium counter cations (N-ethyl-2-(2-methoxyeth...
The urgent need for optimizing the available energy through smart grids and ef cient large-scale energy storage systems is pushing the construction and deployment of Li-ion batteries in the MW range which, in the long term, are expected to hit the GW dimension while demanding over 1000 ton of positive active material per system. This amount of Li-b...
A saturated solution of 2.3 M sodium bis(fluorosulfonyl)imide in trimethyl iso-butyl phosphonium bis(fluorosulfonyl)imide ionic liquid shows a high conductivity (0.94 mScm⁻¹ at 50 °C), low ion association, and a wide operational temperature window (−71 °C–305 °C) making it a promising electrolyte for sodium battery applications. Cycling with P2- an...
Transition metal layered oxides are promising cathode materials for sodium-ion batteries. Phase transitions involving different stacking sequences of the oxide layers often plague the electrochemistry of these materials during cycling, which strongly impacts in their electrochemical performance. However, the underlying mechanisms of these processes...
Olivine NaFePO4 has recently attracted the attention of the scientific community as promising cathode material for Na-ion batteries. In this work we combine density functional theory (DFT) calculations and high resolution synchrotron X-ray diffraction (HRXRD) experiments to study the phase stability of NaxFePO4 along the whole range of sodium compo...
The successful phase separation of P2- and O3-phase Na2/3Fe1/2Mn1/2O2 is demonstrated using co-precipitation method. Although P2-phase displays superior thermodynamic stability at 2/3Na and 1/2Fe:1/2Mn concentration, O3-phase can be stabilized by the means of kinetic control. The electrochemical performance evaluation with half- and full-cells prov...
Local mechanical properties of modified-graphene high-density polyethylene nanocomposites are investigated using depth-sensing indentation. Three different chemical routes are employed to boost filler dispersion by functionalizing graphene with polyethylene brushes and incorporating a small amount of free short-chain polyethylene. At large penetrat...
Here we report the rate capability and cycling stability of NaFePO4 in aqueous electrolyte at various temperatures and voltage windows and compare it to its performance in organic electrolyte under similar conditions. In aqueous electrolyte the polarization was strongly reduced, leading to superior capacity at all tested rates compared to organic e...
We have studied, by small-angle magnetic neutron scattering, the evolution induced by the application of a magnetic field on the coexistence of ferromagnetism and antiferromagnetism in a crystal of Pr0.67Ca 0.33MnO3. The results are compared to magnetic measurements, which provide the evolution of the ferromagnetic fraction. These results show that...
Lithium-ion capacitors (LICs) have attracted an increased attention in the last years. Presently, graphite is the mostly used material for the negative electrodes of LICs. Nevertheless, many works showed that graphite electrodes display rather low performance during high rate charge, as those required for LICs. Therefore the use of alternative carb...
The reaction mechanism occurring during the (de)intercalation of sodium into the host olivine FePO4 structure is thoroughly analysed through a combination of structural and electrochemical methods. In situ XRD experiments have confirmed that the charge and discharge reaction mechanisms are different and have revealed the existence of a solid soluti...
Sodium-ion batteries are considered an attractive
alternative to lithium-ion batteries as could potentially be
much less expensive, safer and environmentally benign
[1]. Similarly to Li-ion cells, in Na-ion batteries Na+ ions
are shuttled between the positive and negative electrodes
during charging and discharging, with an electrolyte
acting as the...
Conventional tests based on immunorecognition and on the use of coloured colloidal particles have still some drawbacks that limit their use: they do not provide a quantitative determination of the analyte, and their sensitivity is limited. Our strategy to overcome these disadvantages consists in the use of superparamagnetic core-shell nanoparticles...
In this paper we examine the mechanism of Na insertion and extraction in the FePO4–NaFePO4 system. Chemical preparation of the intermediate Na1−xFePO4 phase has revealed the existence of a range of stable compositions with different Na+/vacancy arrangements. The mechano-chemical aspects of the charge and discharge reactions are also discussed.
The combination of magnetoresistive sensors and magnetic labeling of bioanalytes, which are selectively captured by their complementary antibody in the proximity of the sensor is a powerful method in order to attain truly quantitative immunological assays. In this paper we present a technical solution to exploit the existing spin valve technology t...
We have studied by small-angle neutron scattering the magnetic field evolution of the magnetic phase separation in a colossal magnetoresistive (CMR) Pr0.7Ca0.3MnO3 crystal, in a wide range of scattering vectors Q , down to 2×10-3Å-1 and up to 10-1Å-1 . Access to such small Q values allows measuring the Q-4 scattering from interfaces between ferroma...
We report a non-linear blue shift of the zero-phonon emission line 5D0→7F0 of Eu3+-dopant in Eu3+-doped nano-glass-ceramics in magnetic field up to 50T. The shift is significantly larger in nano-glass-ceramics compared to its precursor glass, suggesting that the nanoceraming of the precursor glass decreases the effective mass of the f-electrons ban...
The effect of magnetic field on luminescence intensity is generally expected to be rather weak. Contrary to this expectation, we report here an extraordinary strong intensity suppression (by two orders of magnitude) of the Er <sup>3+</sup> <sup>4</sup>S<sub>3/2</sub>→<sup>4</sup>I<sub>15/2</sub> green emission line in Er <sup>3+</sup> -doped nano-g...
Polycrystalline silicon (pc-Si) thin-films with a grain size in the range of 0.1–100 μ m grown on top of inexpensive substrates are economical materials for semiconductor devices such as transistors and solar cells and attract much attention nowadays. For pc-Si, grain size enlargement is thought to be an important parameter to improve material qual...
A bright persistent photoluminescence has been observed in Er(3+)-doped nanoparticles prepared by selective dissolution of bulk oxyfluoride nano-glass-ceramics. A 2 orders of magnitude decrease of intensity of the (4)S(3/2)-->(4)I(15/2) green emission band of Er(3+) in these nanoparticles is observed in magnetic fields up to 50 T. This strong lumin...
The “in situ” preparation and characterization of composites of polyaniline (PANI) and single-walled carbon nanotubes (SWCNTs) are reported. To improve the dispersion and compatibility with the polymer matrix the raw SWCNTs were modified following different routes. SWCNTs oxidized by chemical or thermal treatments (nitric acid and air oxidation, re...
A zero-phonon component of the 1.5 μm emission band of Er3+ in the nano-glass-ceramics 32(SiO2)9(AlO1.5)31.5(CdF2)18.5(PbF2)5.5(ZnF2):3.5(ErF3) mol %, shifts to higher energy and splits into Zeeman doublet in external magnetic field. These effects make it possible to flatten the amplification band of the Er3+-doped amplifier. The blue photoluminesc...
We report on the magnetic properties of the manganite Bi_{1-x}Ca_{x}MnO_3 (x=0.33) at low temperature. The analysis of the field expansion of the ac susceptibility and the observation of aging properties make clear that a spin glass phase appears below T = 39K, in the presence of magnetic order. Neutron scattering shows both magnetic Bragg scatteri...
Small-angle neuron scattering (SANS) magnetic and electrical transport measurements were performed to study a single crystal of Pr0.7Ca0.3MnO3, a colossal magnetoresistive material. While the magnetic-field-induced transformation of this phase separated compound consisting of an antiferromagnetic insulating (AFI) phase and a ferromagnetic insulatin...
Transport properties of manganese oxides suggest that their colossal magnetoresistance (CMR) is due to percolation between ferromagnetic metallic (FM) clusters in an antiferromagnetic insulating (AFI) matrix. We have studied small-angle neutron scattering under an applied magnetic field in CMR Pr1−xCaxMnO3 crystals for x around 0.33. Quantitative a...
This manuscript presents the study by small angles neutron scattering of the magnetic inhomogeneities from nanometric to mesoscopic scales at low temperature in CMR manganite compounds of the series Pr1-xCaxMnO3, x close to 1/3, and its evolution under applied magnetic field.
These systems show a large scale phase separation between a ferromagnetic...
We study the influence of the Joule effect on the nonlinear behavior of the transport I-V curves in polycrystalline samples of the manganite Pr0.8Ca0.2MnO3 by using the crystalline unit-cell parameters as an internal thermometer in x-ray and neutron diffractions. We develop a simple analytical model to estimate the temperature profile in the sample...
Superlattices composed of ferromagnetic Pr0.85Ca0.15MnO3 and ferroelectric Ba0.6Sr0.4TiO3 layers were fabricated on (100) SrTiO3 substrates by a pulsed-laser deposition method. The capacitance and resistive parts of the samples were analyzed from the complex impedance measurements, performed on the samples using a special experimental set-up. The s...
We report a SANS study of the microphase separation texture of a Pr0.66Ca0.33MnO3 crystal as a function of temperature. At TC, ferromagnetic domains display elongated shapes randomly oriented with respect to the crystalline structure, which transform, at lower temperatures, in a texture of randomly oriented and polydisperse 2D sheets of 2nm average...
We have studied by small angle neutron scattering the evolution induced by the application of magnetic field of the coexistence of ferromagnetism and antiferromagnetism in a crystal of Pr0.67Ca0.33MnO3. The results are compared to magnetic measurements, which provide the evolution of the ferromagnetic fraction. These results show that the growth of...
Substitutions at the Mn-site of the charge-ordered Pr0.5Ca0.5MnO3 manganite is an effective way to induce abrupt jumps on the magnetic field driven magnetization curve. In order to get new insights into the origin of this remarkable feature, the Pr0.5Ca0.5Mn0.97Ga0.03O3 perovskite manganite has been studied by neutron diffraction, versus temperatur...
We have studied, by small-angle magnetic neutron scattering, the evolution induced by the application of a magnetic field on the coexistence of ferromagnetism and antiferromagnetism in a crystal of Pr0.67Ca0.33MnO3. The results are compared to magnetic measurements, which provide the evolution of the ferromagnetic fraction. These results show that...
The electrical and magnetic response to a bias current has been investigated in a singlecrystalline ferromagnetic manganese oxide $\Pr_{0.8}$Ca$_{0.2}$MnO$_3$ . A significant decrease of the magnetization is observed at the same threshold current where a non-linearity of V-I characteristics appears. Such a behavior cannot be understood in the frame...
We have investigated the role of the stress induced by the presence of the substrate in thin films of colossal magnetoresistive manganites on structural, resistive, and magnetic properties. Because of the strong coupling between the small structural distortions related to the charge ordering (CO) and the resistive properties, the presence of the su...
11 pages, 6 figures, Presented at the 8th JMMM Conference, San Antonio, Jan 2001. To be published in J. App. Phys
Superlattices composed of ferromagnetic Pr0.85Ca0.15MnO3 and ferroelectric Ba0.6Sr0.4TiO 3 layers were fabricated on (100) SrTiO 3 substrates by a pulsed-laser deposition method. The capacitance and resistive parts of the samples were analyzed from the complex impedance measurements, performed on the samples using a special experimental set-up. The...
Transport properties of the manganese oxides that display a colossal magnetoresistance suggest that it is due to a percolation between ferromagnetic F clusters in an antiferromagnetic AF matrix. We propose to study the evolution of this phase separation at low temperature at the nanometric scale using the small angle neutron scattering in Pr1 xCaxM...