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A high-power and fast charging Li-ion battery with outstanding cycle-life
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Electrochemical energy storage devices based on Li-ion cells currently power almost all electronic devices and power tools. The development of new Li-ion cell configurations by incorporating innovative functional components electrode materials and electrolyte formulations will allow to bring this technology beyond mobile electronics and to boost performance largely beyond the state-of-the-art.
Here we demonstrate a new full Li-ion cell constituted by a high-potential cathode material, i. LiNi 0. TiO 2 , and a composite electrolyte made by a mixture of an ionic liquid suitable for high potential applications, i. Pyr 1,4 PF 6 , a lithium salt, i. LiPF 6 , and standard organic carbonates. Energy conversion and storage are key enabling technologies that will pave the way in the XXI century to mass electro-mobility, smart-grids of continental-size and realistic reduction of CO 2 emissions.
Electrochemical energy storage devices based on Li-ion cells currently power almost all electronic devices. Breakthrough progresses in Li-ion batteries LIBs can be achieved in terms of higher power performance, longer cycle life, improved safety and sustainability 1 by the development of anodes, cathodes and electrolytes materials relying on innovative chemistries 2 , 3.
Here we propose and demonstrate a novel formulation of a full lithium ion cell. The key-innovation stands in the unique combination of a a nanostructure TiO 2 -based negative electrode with a tailored 1-D tubular morphology; b a LiNi 0. This full cell configuration is able to provide outstanding performance in terms of power density and cycling life, in combination with an intrinsically higher safety, compared to commercial cells, provided by the ionic liquid component, and lower costs as well as an improved environmental compatibility due to the absence of cobalt in the cathode material.
In the current literature, a huge number of possible alternative configurations for next generation lithium-ion cells have been proposed, based on a variety of different chemistries at the cathode and anode sides and for the electrolyte 5 , 6 , 7. Among them, the concept of a 3—3. Li ; b titanium oxide-based materials can be easily obtained as nano-particulates by tuning the synthetic conditions, thus disclosing excellent power performance 10 ; their density is two times larger than graphite and therefore the volumetric performance can double compared to a standard graphite-based Li-ion cells Unfortunately, their high operating potential 1.
Thus, they need to be coupled with high-potential cathodes, e. Turning to the cathode side, the high voltage LNMO spinel oxide, is one of the most promising cathode materials due to the large reversible capacity, high thermal stability, low cost and null content of the toxic, high cost and pollutant cobalt The key-point to achieve excellent power performance from this material is the optimization of the synthetic procedure to obtain well-formed particles with optimal morphology However, the adoption of a simple and single-step synthesis strategy to optimize the crystallinity, composition, morphology and surface properties to be able to fully address the serious capacity fading of LNMO cathodes, especially at high rate and at elevated temperatures, has never been reported 3.
In fact, only the combination of a suitable lattice doping with coating layers through complex and expensive multi-stage synthetic procedures is apparently able to lead to materials with superior properties in lithium cells The main reason of the capacity fading of the LNMO electrodes upon cycling roots is in the complex parasitic chemistry that takes place at high potentials onto the positive electrode surface 13 , 14 , It is a matter of fact that the adoption of any high potential positive electrode materials, in combination with commercial carbonate-based electrolytes, results in a massive increase of parasitic reactivity upon cycling above 4.
This unavoidable effect impacts negatively the long-cycling performance and self-discharge, leading to rapid battery failure. Additives and use of non-carbonate based co-solvents have been proposed in the literature 16 , 18 , 19 but, so far, no ultimate solution for stable liquid electrolytes above 4.
Li has been found To address the shortcomings at high potentials outlined above and to improve the safety of the battery we developed a composite solution, made by mixing an ionic liquid IL component, Py 14 PF 6 , with a conventional LiPF 6 -alkyl carbonate based electrolyte i.
The LiPF 6 salt has a unique set of properties for its successful use in lithium battery electrolytes, including the ability to achieve high ionic conductivity and negligible reactivity towards aluminum current collectors. Even though widely adopted, the use of LiPF 6 combined with alkyl carbonate solvents imposes some limitations.
The main issues are the safety hazards related to the volatility of carbonate-components and the limited temperature range for safe and practical ion conduction. Hybridization of volatile carbonates with ionic liquid components was proved to be effective in reducing flammability of the electrolyte 20 , The IL-LP30 composition selected in this work was already introduced by us in ref.
Thus, the coupling of this innovative electrolyte with a high potential positive electrode material, i. LNMO, and an intrinsically safe negative electrode material, i.
TiO 2 , allows a final cell configuration with intrinsic chemical safety comparable with the safest carbonate-based Li-ion cell on market, i. In summary, the here-proposed full lithium ion cell formulation exploits three simultaneous innovations, on the two electrodes sides as well as for the electrolyte, to disclose outstanding and unpreceded power performance and cycling life compared to the state-of-the-art, with a parallel improvement in the intrinsic safety of the device through the use of an ionic liquid component and the full environmental benignity by replacing cobalt in the cathode active material.
LNMO is an iron and chromium doped spinel with the exact stoichiometry Li 0. The X-ray diffraction pattern is shown in Fig. The image shows well-formed prismatic crystallites with sharp edges and regular shape. Figure 1c shows the detail of a particle, demonstrating how the particle is well crystallized in the bulk, while the surface is homogeneously covered by an amorphous 1-to-2 nanometer thick layer.
A more detailed description will be discussed elsewhere. The peak broadening results from the nanoscale of the sample which is also seen in the SEM image, Fig.
Moreover, the TEM image in Fig. The electrochemical performance of the LNMO and TiO 2 -nanotube materials have first been investigated in combination with a standard LP30 electrolyte solution by using half-lithium cells configuration see Methods section.
Electrochemical results are summarized in Fig. On the other hand, the prolonged cycling reversibility may be related to the uniform Cr 2 O 3 amorphous layer on the surface of the particles.
In fact, a beneficial effect of Cr 2 O 3 coatings of the cathode particles at high potential has been predicted by Wolverton and co-workers on the basis of extended density functional theory calculations Compared to the most recent literature available, the here proposed LNMO material outperforms all similar materials in terms of rate capability and extended cycling ability see as an example the very recent review in ref.
The voltage profiles of the TiO 2 -B electrodes half-cell, shown in Fig. The cycling stability of TiO 2 -nanotubes anode was investigated at different current-rates for over cycles.
In the Fig. The specific capacity decay during the first th cycles of Fig. Furthermore, since the high-current rate used the TiO 2 -anode needs more than few cycles for the complete formation of the SEI-layer.
Having established the performance of the negative and positive electrodes in half cells, a full cell configuration was assembled. All the Li-ion batteries here reported have been balanced by matching the cathode and anode capacity. The TiO 2 -B negative electrodes have not been electrochemically activated thank to the chemical mitigation of the irreversible capacity loss in the first cycle obtained by the chemical pre-treatment with lithium ethoxide see the experimental section. For the sake of simplicity, the specific capacity values hereafter reported refer to the LNMO electrode mass.
The voltage profiles shown in Fig. The full-cell shows outstanding performance, comparable to that of the lithium half-cell see and compare Fig. Furthermore, between cycles and , the cell shows a remarkable cycling stability, with capacity only slightly decreasing. The mean working voltage of the cell is 2. Figure 3b gives a further demonstration of the excellent rate performance of this unique Li-ion configuration.
With the new electrolyte the hysteresis between charge and discharge increases at the highest current rates and the profiles become more and more sloping. However, the delivered capacity is almost unaltered. The current rate performance is also excellent, see Fig. Turning to the prolonged cycling performance shown in the Fig. The comparison between the galvanostatic performance of the cell using the pristine LP30 electrolyte and the one using the IL-added highlights minor differences in terms of electrochemical performances, e.
A similar behavior between the full cells is given by the capacity decay during the first th cycles. This can be ascribed to the phenomena occurring at the TiO 2 -anode side related with the SEI formation and further to the partial first irreversible capacity of the cathode material during the first charge. Further comparison reveals that the cell using the IL-added electrolyte has slightly higher Coulombic efficiency than the one using the pristine LP30 electrolyte, thus indicating that the addition of the IL in the LP30 solution is reducing the electrolyte reaction at high voltage.
For better comparison and further discussion see Fig. S1 in the Supplementary Information section. The successful coupling of an Fe- and Cr-doped LNMO spinel and TiO 2 -B nanotubes in Li-ion cells has been demonstrated: this formulation is able to sustain extended cycling and high current rates with minor capacity fade, thus disclosing outstanding performance in terms of energy and power capability, as well as in terms of long calendar life.
Such excellent performance are confirmed both in a standard carbonate-based electrolyte and in an innovative composite electrolyte modified by the addition of a stable ionic liquid, aimed at the improvement of the overall safety of the battery. The LNMO electrode material here discussed differs from the state-of-art reported due to the unique synergic role played by the simultaneous iron doping and Cr-oxide coating.
This composition tuning improves the structural stability, the electronic conductivity and prevents the electrolyte decomposition at high-voltage and C-rates. The final effect is the development of an electrode material having high cycling stability and excellent rate capability, prepared with an easy scalable and cheap synthetic route.
Moreover, the unique morphology of this negative electrode material allows excellent rate performance and extended calendar life with minor capacity loss upon cycling. S2 and related discussion in the Supplementary Information section. Furthermore, the Li-ion cell here developed showed an outstanding cycle-life, exceeding thousands cycles. With this work we marked a step forward in the field of future Li-ion battery, since the device here developed shows C-rates, energy performance and cycle-life never reported before.
Doped LiNi 0. Then the product of the hydrothermal reaction was washed with 0. After the annealing the synthesized TiO 2 B material has been transferred directly to the glove box without exposure in air. Before casting into film electrodes, the TiO 2 -B material has been treated with lithium ethoxide following the procedure illustrated by Brutti and co-workers in ref. The preparation of the TiO 2 B based electrode films has been carried out in glove box to avoid the possible contamination with moisture.
Galvanostatic cycling tests at different current rates were carried out with a Maccor series battery tester, using voltage range between 5V—2. The Full Li-ion cell started in charge and cycled in the voltage range 4. No electrochemical pre-activation on both the electrodes was carried out before cycling.
Larcher, D. Towards greener and more sustainable batteries for electrical energy storage. Chem 7 , 19—29, doi: Hassoun, J. Kraytsberg, A.
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