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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Hydroxide melt induced corrosion of Ni at elevated temperatures under steam electrolysis conditions

Molten alkali electrolyte based high temperature water electrolysis (HTWE) process offers an efficient pathway to integrate renewable energy resources for large scale and economic hydrogen production. Long term and stable operation of these systems require an in-depth understanding of materials stability under anodic and cathodic exposure conditions of the cell and cell stacks. In the present study, we report our findings on the corrosion of Ni in the presence and absence of (LieNa) hydroxide melt at 600 °C under oxidizing and reducing conditions representative of HTWE. While the Ni electrode was found to remain thermodynamically stable in metallic form under cathodic (reducing) exposure conditions, the corrosion rate in molten hydroxide under oxidizing conditions was found to be nonparabolic in nature. A cyclic voltammetry study provides the breakdown of the passive metal-oxide surface layer at the anodic overpotential region between 0.45 V and 2 V in molten hydroxide under oxidizing conditions. As a result, a thermochemical process for accelerated corrosion based on the oxide scale fluxing in hydroxide melt has been developed.

08 HYDROGEN↗
DOE OSTI2024

Trace Fe activates perovskite nickelate OER catalysts in alkaline media via redox-active surface Ni species formed during electrocatalysis

The accurate description of activity trends among perovskite-oxide oxygen-evolution-reaction (OER) catalysts using electronic-structure descriptors requires that the bulk structure of the catalyst is comparable to that of the surface. Few studies have addressed the dynamic nature of the catalyst's structure during the OER and the consequential implications for understanding activity. Here, we use a combination of electrochemical and materials-characterization techniques to study the surface reconstruction and the associated formation of a new redox-active phase on LaNiO 3 particles, LaNiO 3 epitaxial films, and an analogous Ruddlesden-Popper phase, La 2 NiO 4 . Small, but characteristic, redox features corresponding to Ni redox in nominally amorphous NiO x H y are observed during cyclic voltammetry of these initially fully crystalline materials. The size of these redox features grows with prolonged cycling and contributes to an increased surface area as determined from electrochemical impedance spectroscopy (EIS). Here we find the OER activity is strongly dependent on soluble Fe species in the electrolyte, common impurities in alkaline media. These observations are consistent with the reconstruction of the crystalline surface to form NiO x H y species and subsequent activation by adsorption of Fe forming the well-known and extremely active NiFeO x H y OER catalyst.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Electrochemical generation of hexacyanoferrate and hexacyanoruthanate electroactive films at nickel electrode surfaces: A promising synthetic approach for new electrode materials in metal ion batteries and supercapacitors

Prussian blue analogues (PBAs) have been recently investigated as promising electrode materials for battery and supercapacitor applications. While most explorations have focused on PBA nanoparticles, very little attention has been focused on PBA films deposited on a metallic support. In this work, we have examined electrogenerating hexacyanoferrate (HCF) and hexacyanoruthenate (HCR) films on nickel surfaces via cyclic voltammetry. We found that the total material deposited was influenced by the metal cation present in the electrolyte solution and that, on average, the rate of deposition of the surface adsorbed/immobilized species was dependent on the species in solution. In particular, films electrogenerated in the presence of Na + and K + had the highest deposition rates. The cyclic voltammetric profiles exhibited dramatic differences depending on the cation present in the electrolyte solution. In addition, we found that all films were electrochemically irreversible in the presence of Li + and Mg 2+ containing electrolyte solutions. Further, and as a proof of concept, we modified high surface area nickel electrodes with HCF in sodium-based electrolytes, finding that these electrodes could operate reversibly at equivalent C-rates as high as 1667C.

25 ENERGY STORAGE↗
DOE OSTI2021

Tracking the evolution of processes occurring in silicon anodes in lithium ion batteries by 3D visualization of relaxation times

An unconventional electroanalytical method has been used for tracking processes in silicon anodes in lithium ion batteries: a 3D visualization of relaxation times. Impedance data of the electrodes were collected at different potentials and different cycles during cyclic voltammetry, and were treated by means of the Distribution of Relaxation Times (DRT) method. A 3D visualization of the results allowed to identify the formation of a solid electrolyte interphase on the anode, composed of two layers with different relaxation times. Such findings are not possible by conventional analysis of impedance data by modeling with equivalent circuits, nor by simple DRT alone. Additionally, it was possible to observe that the characteristic relaxation time of the lithiation of the Si anode becomes smaller upon cycling, indicating that the material experiences structural transformations that allow it to lithiate faster. The result is relevant to motivate the use of micron-sized particles in the anode.

25 ENERGY STORAGE↗
DOE OSTI2023

Electrochemical properties of Gd(III) ions in LiCl-KCl-GdCl 3 at 723–1023 K

Electrochemical behavior of Gd(III) ions in molten LiCl-KCl-GdCl 3 was investigated at 723–1023 K via cyclic voltammetry using tungsten as a working electrode, Gd-Bi (mole fraction, x Gd = 0.16) as a reference electrode, and Gd-Bi (x Gd = 0.02) as a counter electrode. A single reduction–oxidation wave was observed, confirming a single-step, 3-electron transfer Gd(III)/Gd transition. The cathodic peak potential exhibited minimal change (<13 mV) over a wide range of scan rates (0.05–0.30 V s –1 ), indicating facile charge transfer kinetics (i.e., a reversible electrode process). A nucleation overpotential associated with solid Gd deposition was observable at low temperatures (T < 823 K). The mass transport properties of Gd(III) ions were estimated using the Berzins and Delahay relation based on diffusion-limiting peak current. The diffusivity values were determined to be D Gd(III) = 0.5–2.7 × 10 –5 cm 2 s –1 at 723–1023 K with an associated activation energy of E a = 33.9 (±1.0) kJ mol –1 . Finally, the two-phase [liquid + GdBi] Gd-Bi alloy reference electrode experienced less than 0.5 mV of drift over 5 days of repeated electrochemical measurements, indicating high stability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Precious metal oxygen-evolving anodes for electrolytic reduction of metal oxides in molten LiCl-Li 2 O electrolyte

Understanding the electrochemical stability of oxygen-evolving anode materials in molten salt electrolytes is essential to enable decarbonized electrolytic reduction of metal oxides (e.g., used nuclear oxide fuels). Here, this work investigated three precious metals (Ir, Ru, and Pt) as oxygen-evolving anodes in molten LiCl-Li 2 O (99.0-1.0 wt%) at 650 °C. For consistent measurements, this work employed a three-electrode cell comprised of a two-phase Li-Bi (65-35 at%) reference electrode and a NiO counter electrode. Anodic polarization behavior of each anode was investigated via cyclic voltammetry (CV) and chronoamperometry. The onset potential for oxygen evolution was observed at E > 2.9 V (vs. Li/Li + ) for the Ir and Ru anodes and anodic current density was as high as 1.0 A cm -2 at 3.23 V. The dimensional stability of each anode was evaluated from long-term electrolysis experiments (10.0-32.1 h) at 3.23 V. Rapid consumption of the Pt anode was observed after the application of 26,453 C cm -2 with a reduction in diameter of about 15.8% due to the formation of a non-protective Li 2 PtO 3 compound. The formation of this compound was also observed during CV measurements as additional anodic waves at potentials more negative than that of oxygen evolution. In contrast, both the Ir and Ru anodes exhibited excellent dimensional stability with a reduction in diameter or thickness of less than 1.5% even after applying greater charge density of ~41,100 C cm -2 , demonstrating superior stability during oxygen evolution in the LiCl-Li 2 O electrolyte.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Structural and Biophysical Properties of a [4Fe-4S] Ferredoxin-Like Protein from Synechocystis sp. PCC 6803 with a Unique Two Domain Structure

Electron carrier proteins (ECPs), binding iron-sulfur clusters, are vital components within the intricate network of metabolic and photosynthetic reactions. They play a crucial role in the distribution of reducing equivalents. In Synechocystis sp. PCC 6803, the ECP network includes at least nine ferredoxins. Previous research, including global expression analyses and protein binding studies, has offered initial insights into the functional roles of individual ferredoxins within this network. This study primarily focuses on Ferredoxin 9 (slr2059). Through sequence analysis and computational modeling, Ferredoxin 9 emerges as a unique ECP with a distinctive two-domain architecture. It consists of a C-terminal iron-sulfur binding domain and an N-terminal domain with homology to Nil-domain proteins, connected by a structurally rigid 4-amino acid linker. Notably, in contrast to canonical [2Fe-2S] ferredoxins exemplified by PetF (ssl0020), which feature highly acidic surfaces facilitating electron transfer with photosystem I reaction centers, models of Ferredoxin 9 reveal a more neutral to basic protein surface. Using a combination of electron paramagnetic resonance spectroscopy and square-wave voltammetry on heterologously produced Ferredoxin 9, this study demonstrates that the protein coordinates 2x[4Fe-4S]2+/1+ redox-active and magnetically interacting clusters, with measured redox potentials of -420 +/- 9 mV and -516 +/- 10 mV vs SHE. A more in-depth analysis of Fdx9's unique structure and protein sequence suggests that this type of Nil-2[4Fe-4S] multi-domain ferredoxin is well conserved in cyanobacteria, bearing structural similarities to proteins involved in homocysteine synthesis in methanogens.

cyanobacteria↗
DOE OSTI2025

Differential Ligation Alters Electronic State and Coupling Signals of Iron-Sulfur Clusters in Flavin-Based Electron Bifurcation

Flavin-based electron bifurcation (FBEB) is employed by microorganisms for controlling pools of redox equivalents by reversibly splitting electron pairs into high- and low-energy levels from an initial midpoint potential. Our ability to harness this phenomenon is crucial for biocatalytic design which is limited by our understanding of energy coupling in the bifurcation system. In Pyrococcus furiosus, FBEB is carried out by the NADH-dependent ferredoxin:NADP+-oxidoreductase (NfnSL), coupling the uphill reduction of ferredoxin in NfnL to the downhill reduction of NAD+ in NfnS from oxidation of NADPH. Flanking the bifurcating flavin are two site-differentiated iron-sulfur clusters; the nearest is a glutamate-ligated [4Fe-4S] cluster in NfnL. Recent biochemical experiments substituting the native glutamate with cysteine led to loss of coupling between the uphill and downhill pathways, in contrast to the tight thermodynamic coupling in the native system. To understand how this decoupling is biochemically manifested by the cysteine-substituted [4Fe-4S] in NfnL, we employed electron paramagnetic resonance (EPR) spectroscopy to identify changes in electronic architecture and square wave voltammetry (SWV) to probe thermodynamic shifts produced by the substitution. We observed notable g-value shifts in the EPR for the cysteine-substituted iron-sulfur cluster in addition to significant downward shifts in the redox potential, as well as the disappearance of several low-field signals observed in the native NfnSL complex. These results suggest the site-differentiated glutamate residue facilitates higher spin states in the [4Fesingle bond4S] cluster to bridge energetic gaps in electron transfer to the bifurcating flavin in the native complex, preventing unwanted short-circuiting seen in the cysteine-substituted complex.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Electrochemical behavior and separation of iodide in molten LiF-NaF-KF melt

This work studied the electrochemical behavior of iodide in molten LiF-NaF-KF mixture and the separation of iodide from the molten salt at 973 K using a graphite working electrode. The cyclic voltammetry (CV) and chronoamperometry (CA) measurements indicated an anodic passivation layer was formed on the graphite electrode in this melt and the layer blocked the charge transfer across the electrolyte/electrode interface. However, the added I- ions could pass through the passivation layer and were oxidized at the graphite electrode. The characterization of the obtained products proved that iodide ions was efficiently oxidized to I2 gas during electrolysis. Furthermore, the graphite anode showed excellent stability without any obvious change in dimensions after electrolysis, which showed the high current efficiency of I2 evolution reaction. Thus, the graphite electrode was possible to be served as an excellent anode to separate other anions (such as Br) from molten fluoride salts.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Synthesis and characterization of the dinuclear cobalt(III) complex: [(C 2 F 5 ) 3 Co(μ-F)] 2 2–

Here, reaction of the versatile tris(perfluoroethyl) cobalt(III) precursor [fac-(MeCN) 3 Co(C 2 F 5 ) 3 ] with [NMe 4 ]F and [PPh 4 ]Cl in THF formed the unexpected cobalt(III) bridging fluoride dimer ([(C 2 F 5 ) 3 Co(μ-F)] 2 2– . The new fluoro-organometallic cobalt(III) complex was characterized by NMR and UV-vis spectroscopies, X-ray crystallography, cyclic voltammetry, and by computational methods. In the strongly coordinating solvent MeCN, ([(C 2 F 5 ) 3 Co(μ-F)] 2 2– exhibits dynamic processes on the NMR timescale which are consistent with solvent coordination. However, in the weakly coordinating solvent CH 2 Cl 2 , a more static structure is observed suggesting that the dimer retains its structure in solution state. An electrochemical analysis of ([(C 2 F 5 ) 3 Co(μ-F)] 2 2– was performed, and the data are compared to previously reported cobalt(III) perfluoroethyl complexes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Operando Revealing Dynamic Reconstruction of NiCo Carbonate Hydroxide for High-Rate Energy Storage

Transition metal carbonate hydroxide (CH) has been widely explored as a promising battery-type electrode for high-rate energy storage. However, its genuine active sites under realistic operating conditions remains elusive. In this work, by virtue of the cutting-edge operando X-ray absorption spectroscopy, we unfold the dynamic evolution of the local electronic and geometric structures for the CH electrode upon cycling. Our results reveal that the irreversible redox of Co cations at the early stage of cyclic voltammetry (CV) cycling induces a phase transition in the NiCo CH nanowires forming oxygen vacancies-enriched NiCo layered double hydroxide (LDH) nanosheets with superior high-rate energy storage ability. Theoretical modeling demonstrates that the unsaturated 5-coordinated Co sites exhibit optimal redox reaction energy barrier and immensely promote the performance. These findings not only elucidate the electrochemical susceptibility of the Co-based carbonate hydroxide under operando conditions, but also highlight an electrochemical coordination-engineering strategy for the rational design of high-performance electrode.

25 ENERGY STORAGE↗
DOE OSTI2020

LiNi x Fe y Al z O 2 , a new cobalt-free layered cathode material for advanced Li-ion batteries

Recently, rapid fluctuations in cobalt prices have created a worsening supply chain constraint that has become a serious cause of concern amidst global battery manufacturers. To address this challenge, we report herein a new class of cobalt-free, nickel-rich layered cathode material termed the NFA class with general formula LiNi x Fe y Al z O 2 (x + y + z = 1). Using co-precipitation reaction in a continuous stirred tank reactor, we synthesized NFA(OH) 2 precursors with the constituent Ni, Fe and Al elements successfully incorporated. The obtained LiNFAO 2 cathode was characterized using X-Ray diffraction, Mössbauer spectroscopy and scanning electron microscopy. Electrochemical behavior was assessed using cyclic voltammetry, galvanostatic charge/discharge, electrochemical impedance spectroscopy and galvanostatic intermittent titration technique at various states of lithiation/delithiation. Electrochemical performance evaluations revealed that our cobalt-free material delivers high capacity of 190 mAh/g at 0.1C. Rate and cycling performance evaluations also indicated good rate capability and cycling stability with 88% capacity retention after 100 cycles at C/3. Using NFA cathodes, we also fabricated a 0.5Ah (C/3) cobalt-free Li-ion battery which demonstrated reasonable cycling stability with ~72% capacity retained after 200 cycles. Overall, our work demonstrates the immense potential of the cobalt-free NFA class cathodes as viable candidates towards development of next generation cost effective lithium ion batteries.

25 ENERGY STORAGE↗
DOE OSTI2022

Calorimetry can detect the early onset of hydrolysis in hybrid supercapacitors with aqueous electrolytes

This study investigates the effect of cation species on the onset of electrolyte hydrolysis in hybrid supercapacitors with aqueous electrolytes using isothermal operando calorimetry. The cells consisted of a positive α-MnO 2 cryptomelane electrode and a negative activated carbon (AC) electrode with either 0.5 M K 2 SO 4 or 0.5 M Cs 2 SO 4 aqueous electrolytes. They were characterized using cyclic voltammetry and galvanostatic cycling. In addition, the instantaneous heat generation rate at each electrode was measured using a custom isothermal operando calorimeter. Heat generation associated with resistive losses (Joule heating) and reversible ion adsorption/desorption was clearly identified. For larger potential windows, an endothermic dip, attributed to the onset of hydrolysis, was observed at the positive α-MnO 2 electrode where K + and Cs + ions engaged in fast surface redox reactions. Interestingly, this endothermic dip appeared at 1.8 V and 2.0 V for K 2 SO 4 and Cs 2 SO 4 aqueous electrolytes, respectively. The difference in the stable operating potential window was attributed to thinner solvation shell around Cs + cation than for K + thus reducing the amount of water present near the electrodes as ions partially shed their solvation shells during adsorption. The early onset of hydrolysis could be observed by isothermal operando calorimetry before it could be observed with conventional electrochemical methods.

42 ENGINEERING↗
DOE OSTI2023

Improving charge transport in integrated MoO 3 /C electrode materials for water-in-salt energy storage systems by incorporating oxygen vacancies

Improvements in the charge storage properties of α-MoO 3 used as an electrode with a 30m ZnCl 2 water-in-salt electrolyte have been achieved by enhancements in electron and ion transport enabled by an inventive synthesis route. Electron transport was improved through the integration of MoO 3 with dopamine-derived carbon via a chemical preintercalation route, and enhanced ion transport was achieved by incorporating oxygen vacancies in MoO 3 structure through ethanol 2 reduction under hydrothermal conditions. Here, the presence of carbon was confirmed by corresponding D and G bands observed in Raman spectroscopy measurements. The presence of oxygen vacancies was proven through correlated XPS, TGA, Raman spectroscopy and XRD analyses, with the introduction of oxygen vacancies leading to an expanded interlayer region. Four-point probe measurements provided evidence of increased electronic conductivity due to the incorporation of carbon, and cyclic voltammetry-based charge storage mechanism analyses revealed increases in ion transport kinetics due to oxygen vacancy formation. Tuning the oxygen vacancy concentration is critical, as excessive concentrations of these point defects leads to structural instability and poor capacity retention. This work demonstrates the combined potential of carbon and oxygen vacancies in moderate concentrations to enhance the charge storage properties of transition metal oxides. The strategies developed in this study offer a path to the development of promising materials for high-rate, high-capacity, and long-duration electrochemical energy storage technologies.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2025

Assessing the coating implications of slurry formulations in NCMA and LFMP blend cathodes for lithium-ion batteries

This paper investigates the implications of slurry formulations and electrode processing on the performance of lithium-ion battery (LIB) cathodes, focusing on Nickel Cobalt Manganese Aluminum (NCMA) and Lithium Ferro Manganese Phosphate (LFMP) blends. Through a comprehensive examination of electrode processing steps, from material selection to coating application, we elucidate the critical role of processing parameters in shaping electrode morphology and electrochemical behavior. Rheological studies reveal the influence of slurry composition on viscosity and flow behavior, highlighting the importance of achieving optimal rheological properties for uniform coating deposition. Electrochemical characterization, including cyclic voltammetry and rate capability tests, unveils the electrochemical behavior of NCMA, LFMP, and their blend, showcasing the synergistic effects of material blending on battery performance. In conclusion, our findings underscore the intricate relationship between slurry formulation, electrode processing, and LIB performance, offering valuable insights for the design and optimization of high-performance electrode materials for next-generation batteries.

25 ENERGY STORAGE↗
DOE OSTI2026

Tetrahedral Zn 2+ doping LiNi 0.6 Mn 0.2 Co 0.2 O 2 improves discharge capacity retention by altering surface Ni valence during cycling and preventing oxygen evolution

5 mol-% Zn 2+ was added to the co-precipitation synthesis of LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) to understand Zn's effect on the structural and electronic properties of NMC622. Zn is determined to successfully dope into the NMC crystal lattice as there is an increase in d-spacing along the [003], [104], and [110] directions and an increase in molar volume (100.75 cm 3 mol -1 for NMC622 and 101.00 cm 3 mol -1 for Zn-NMC). Through XPS, Zn is determined to dope on the tetrahedral 6c Wyckoff site in the NMC structure and TEM-EDS reveals that despite a slight ZnO impurity phase, 1.4 mol-% Zn successfully dopes into the crystal structure. Furthermore, cyclic voltammetry shows a suppressed anodic wave associated with oxygen evolution and EIS demonstrates that Zn-doped NMC decreases charge transfer resistance and increases Li diffusion by an order of magnitude. After the formation cycles, NMC has a higher 1 C accessible capacity, 141 mAh/g, over Zn-NMC (132 mAh/g), but after long term cycling Zn-NMC has a higher accessible capacity (117 mAh/g compared to 96 mAh/g for NMC) and increases discharge capacity retention by 18% leading to longer cycle life.

Electrochemistry↗
DOE OSTI2023

Oxide derived Cu nanofibril assembly for enhanced nonenzymatic glucose sensing

In this report, we have prepared copper nanofibril assembly via thermal oxidation followed by electrochemical reduction processes, exhibiting superior glucose detection ability. The morphological analysis evidenced the formation of rough islands or nanofibril structure on the Cu surface depending on initial thermal oxidation temperature. The glucose detection performance was investigated by performing cyclic voltammetry and chronoamperometry with varying glucose concentration. A high sensitivity (4131.57 μA mM – 1 cm – 2 ), low detection limit (1.41 μM), wider linear range (0–3.9 mM) and long–term stability (30 days) have been recorded for electrode thermally oxidized at 400 °C followed by electrochemical reduction process (rCu_400). The sensitivity is almost three times higher in comparison to the planner Cu surface. This significantly enhanced glucose sensing ability rCu_400 has been attributed to the nanofibril morphology, origination of Cu (111) facet and formation of a stable oxide layer evidenced by scanning electron microscopy, X-ray diffraction and energy dispersive spectroscopy analysis. Despite higher sensitivity, rCu_400 electrode does not show any response to the chloride ion, dopamine, ascorbic acid and uric acid. Finally, these results indicate that the Cu nanofibril structure prepared via simple oxidation/reduction process can be an excellent candidate to be used as an electrode for glucose sensing application.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Improving the bulk gas transport of Fe-N-C platinum group metal-free nanofiber electrodes via electrospinning for fuel cell applications

To overcome transport limitations associated with thicker platinum group metal-free (PGM-free) electrodes, it's essential to investigate and tailor alternative electrode architectures to maximize the bulk electrode transport properties, whilst not significantly impeding electrocatalyst active site accessibility and electrode proton resistance. In this work, PGM-free nanofiber electrode mats, prepared by electrospinning a mixture of pyrolyzed Fe-N-C catalyst, Nafion ionomer and a carrier polymer Poly Acrylic acid (PAA), were compared to traditionally prepared electrodes. The morphological properties and elemental distribution of the fabricated nanofiber electrodes showed that the exterior surface of the PGM-free nanofibers was conformally covered with a thin ionomer film. Electrochemical diagnostics performed utilizing cyclic voltammetry, electrochemical impedance spectroscopy (EIS) and H 2 -limiting current measurements, revealed an increase in electric double layer capacitance, reduction in electrode proton transport and a significant improvement in bulk-electrode gas transport properties for the nanofiber electrodes, supporting the observed performance increase from electrochemical polarization data obtained in H 2 -O 2 /Air fuel cells. At 100% RH in H2/Air, the power density of the nanofiber electrodes increased ca. 50% vs. the traditionally prepared electrodes (ca. 260 vs 175 mW cm -2 ), which was attributed to a less tortuous molecular diffusion pathway and an associated reduction in the pressure dependent and independent gas transport resistances in the nanofiber electrodes.

25 ENERGY STORAGE↗