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Efficiency and Quality Issues in the Production of Black Phosphorus by Mechanochemical Synthesis: A Multi-Technique Approach
摘要： Black phosphorus (BP) is a two-dimensional material potentially of great interest for applications in the fields of energy, sensing, and microelectronics. One of the most interesting methods to obtain BP is the conversion from red phosphorus (RP) by means of high-energy mechanochemical synthesis. To date, however, this synthesis process was not well characterized. In this work, starting from the mathematical model of energy transfer during the ball milling process, we investigate the effects on RP → BP conversion of three experimental parameters, the rotation speed, the milling time, and the weight ratio between the spheres and the milled material (BtPw ratio). The efficiency of the conversion process was verified by solid-state NMR, Raman spectroscopy, and X-ray diffraction. Whereas the first two parameters have a minor importance, the BtPw ratio plays a primary role in the RP → BP conversion. Yields approaching 100% can be obtained also with short milling times (15 min) and adequate rotation speed (e.g., 500 r.p.m.), provided that the BtPw ratio >40:1 is used. These results confirm the energy sustainability of the mechanochemical synthesis approach.
关键词： diffraction,solid-state NMR,anode,post-lithium ion batteries,Raman,mechanochemical synthesis
更新于2025-11-21 11:18:25
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Nanoparticle Emissions from Metal-Assisted Chemical Etching of Silicon Nanowires for Lithium Ion Batteries
摘要： As one of the most promising anode materials for high-capacity lithium ion batteries (LIBs), silicon nanowires (SiNWs) have been studied extensively. The metal-assisted chemical etching (MACE) is a low-cost and scalable method for SiNWs synthesis. Nanoparticle emissions from the MACE process, however, are of grave concerns due to their hazardous effects on both occupational and public health. In this study, both airborne and aqueous nanoparticle emissions from the MACE process for SiNWs with three sizes of 90 nm, 120 nm, and 140 nm are experimentally investigated. The prepared SiNWs are used as anodes of LIB coin cells, and the experimental results reveal that the initial discharge and charge capacities of LIB electrodes are 3636 and 2721 mAh g-1 with 90 nm SiNWs, 3779 and 2712 mAh g-1 with 120 nm SiNWs, and 3611 and 2539 mAh g-1 with 140 nm SiNWs. It is found that, for 1 kW h of LIB electrodes, the MACE process for 140 nm SiNWs produces a high concentration of airborne nanoparticle emissions of 2.48 × 109 particles/cm3; the process for 120 nm SiNWs produces a high mass concentration of aqueous particle emissions, with a value of 9.95 × 105 mg/L. The findings in this study can provide experimental data of nanoparticle emissions from the MACE process for SiNWs for LIB applications, and can help the environmental impact assessment and life cycle assessment of the technology in the future.
关键词： Lithium ion batteries (LIBs),Metal-assisted chemical etching (MACE),Nanoparticle emissions,Silicon nanowires (SiNWs)
更新于2025-09-23 15:23:52
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Temperature fiber sensing of Li-ion batteries under different environmental and operating conditions
摘要： In this work, a network of fiber sensors has been developed for real time, in situ, and in operando multipoint monitoring the surface temperature distribution on a smartphone Li-ion battery (LiB). Different temperature and relative humidity conditions are considered, in order to mimic the LiB response in the dry, temperate, and cold climates. In total, the temperature variations that occur in five different locations of the LiB are monitored, during constant current charge and different discharge rates, under normal and abusive operating conditions, performing a thermal spatial mapping of the battery surface. In general, the sensors detect temperature variations according to the voltage signal change and faster variations of voltage usually translate in higher temperature rise at the LiB surface. For instance, under abusive discharge, where the voltage drop is fast, the temperature increases at least twice when compared to the normal operating conditions. Absolute temperature values as high as (65.0 ± 0.1) °C are detected by the optical sensor located near the electrodes, under the higher discharge rate (5.77 C) and dry climate. A thermal gradient is identified from the top to the bottom on the LiB surface during the experimental tests. A lower battery performance is observed when it operates under the cold climate, with maximum temperature variations of (30.0 ± 0.1) °C for the higher discharge rate. These results can be helpful to design of next generation of LiBs, improving a faster cooling in critical areas, in order to reduce accumulated heat and preventing consequences such as thermal runaway and failure.
关键词： Fiber Bragg grating sensors,Temperature monitoring,Abnormal operating conditions,Environment,Safety,Li-ion batteries
更新于2025-09-23 15:23:52
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Acetic anhydride as oxygen donor in the non-hydrolytic sol-gel synthesis of mesoporous TiO2 with high electrochemical lithium storage performances
摘要： An original, halide-free non-hydrolytic sol-gel route to mesoporous anatase TiO2 with hierarchical porosity and high specific surface area is reported. This route is based on the reaction at 200 °C of titanium (IV) isopropoxide with acetic anhydride, in the absence of a catalyst or of a solvent. NMR studies indicated that this method provides an efficient, truly non-hydrolytic and aprotic route to TiO2. Formation of the oxide involves acetoxylation and condensation successive reactions, both with ester elimination. The resulting TiO2 materials were nanocrystalline, even before calcination. Small (≈10 nm) anatase nanocrystals spontaneously aggregated to form mesoporous micron sized particles with high specific surface area (260 m2 g-1 before calcination). Evaluation of the lithium storage performances showed a high reversible specific capacity, particularly for the non-calcined sample with the highest specific surface area favoring pseudo-capacitive storage: 253 mAh g-1 at 0.1C and 218 mAh g-1 at 1C (C = 336 mA g-1). This sample also showed good cyclability (>92% retention after 200 cycles at 336 mA g-1) with a high coulombic efficiency (99.8 %). Synthesis in the presence of a solvent (toluene or squalane) offers the possibility to tune the morphology and texture of the TiO2 nanomaterials.
关键词： anatase,mesoporous,acetic anhydride route,non-hydrolytic sol-gel,Li-ion batteries
更新于2025-09-23 15:23:52
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Easy preparation of nanoporous Ge/Cu3Ge composite and its high performances towards lithium storage
摘要： Nanoporous Ge/Cu3Ge composite is fabricated simply through selective dealloying of GeCuAl precursor alloy in dilute alkaline solution. The as-made Ge/Cu3Ge is characterized by three dimensional (3D) bicontinuous network nanostructure which comprises of substantial nanoscale pore voids and ligaments. Owing to the 3D porous architecture and the introduction of well-conductive Cu3Ge, the lithium storage performances of Ge are dramatically enhanced in terms of higher cycling stability and superior rate performance. Nanoporous Ge/Cu3Ge anode delivers steady capacities above 1000 mA h g-1 upon cycling for 70 loops at 400 mA g-1. In particular, after 300 cycles at the high rate of 3200 mA g-1 the capacity retention for Ge/Cu3Ge is able to reach a maximum of 99.3%. On the contrary, the pure nanoporous Ge encounters severe capacity decay. In view of the outstanding energy storage performances and easy preparation, nanoporous Ge/Cu3Ge exhibits great application potential as an advanced anode in lithium storage related technologies.
关键词： dealloying,anode,lithium ion batteries,nanoporous,germanium
更新于2025-09-23 15:23:52
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GeO <sub/>2</sub> Encapsulated Ge Nanostructure with Enhanced Lithium-Storage Properties
摘要： Germanium (Ge)-based nanostructures, especially those with germanium dioxide (GeO2), have drawn great interest for applications in lithium (Li)-ion batteries due to their ultrahigh theoretical Li+ storage capability (8.4 Li/Ge). However, GeO2 in conventional Ge(s)/GeO2(c) (where (c) means the core and (s) means the shell) composite anodes with Ge shell outside GeO2 undergoes an irreversible conversion reaction, which restricts the maximum capacity of such batteries to 1126 mAhg?1 (the equivalent of storing 4.4 Li+). In this work, a porous GeO2(s)/Ge(c) nanostructure with GeO2 shell outside Ge cores are successfully fabricated utilizing the Kirkendall effect and used as a lithium-ion battery anode, giving a substantially improved capacity of 1333.5 mAhg?1 at a current density of 0.1 Ag?1 after 30 cycles and a stable long-time cycle performance after 100 cycles at a current density of 0.5 A g?1. The enhanced battery performance is attributed to the improved reversibility of GeO2 lithiation/delithiation processes catalyzed by Ge in the properly structured porous GeO2(s)/Ge(c) nanostructure.
关键词： porous,Kirkendall effect,nanostructures,lithium ion batteries,GeO2(s)/Ge(c)
更新于2025-09-23 15:22:29
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One-pot Hydrothermal Synthesis of ZnO Microspheres/Graphene Hybrid and its Electrochemical Performance
摘要： In this paper, the ZnO microspheres/graphene hybrids were successfully prepared from zinc acetate and GO aqueous solution by a facile one-pot hydrothermal method without any surfactant. The as-synthesized samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), thermogravimetric (TGA) analysis, nitrogen adsorption/desorption isotherms and pore size distribution. When evaluated as anode material for lithium ion batteries, it delivered a high initial discharge capacity of 1150 mAh g-1 and exhibited excellent rate performance at different current densities.
关键词： anode materials,ZnO microspheres/graphene hybrid,one-pot hydrothermal,lithium ion batteries
更新于2025-09-23 15:21:01
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Preparation of Highly Oriented Porous LiCoO2 Crystal Films via Li-Vapor Crystal Growth Method
摘要： To construct better Li-ion-based batteries, highly oriented porous LiCoO2 crystal film is urgently needed for an active positive electrode. In this study, we prepared such a crystal film via the Li-vapor crystal growth method, which involves a simple reaction between the CoO substrate and Li-vapor. Highly crystalline LiCoO2 particles 2–3 μm in size were grown on the CoO substrate surface with strong relation of their orientation. The <110> and <018>-oriented LiCoO2 particles, which are preferable for Li-ion conduction, were generated on the CoO(110) substrate. On the CoO(111) substrate, LiCoO2 particles were grown with not only the <003> orientation but also the <012> orientation, suggesting that the crystal growth should follow the three-dimensional structure of the CoO and LiCoO2 lattice. Both the prepared LiCoO2 films from the CoO(110) and CoO(111) substrates exhibited stable and superior electrochemical properties for Li-ion battery cycling, indicating that the films will be useful for high-performance Li-ion-based batteries.
关键词： highly oriented porous film,LiCoO2 electrode,Li-vapor crystal growth,Li-ion batteries
更新于2025-09-23 15:21:01
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Ultrathin two-dimensional conjugated metala??organic framework single-crystalline nanosheets enabled by surfactant-assisted synthesis
摘要： Two-dimensional conjugated metal-organic frameworks (2D c-MOFs) have recently emerged for potential applications in (opto-)electronics, chemiresistive sensing, and energy storage and conversion, due to their excellent electrical conductivity, abundant active sites, and intrinsic porous structures. However, developing ultrathin 2D c-MOF nanosheets (NSs) for facile solution-processing and integration into devices remains a great challenge, mostly due to unscalable synthesis, low yield, limited lateral size and low crystallinity. Here, we report a surfactant-assisted solution synthesis toward ultrathin 2D c-MOF NSs, including HHB-Cu (HHB=hexahydroxybenzene), HHB-Ni and HHTP-Cu (HHTP=2,3,6,7,10,11-hexahydroxytriphenylene). For the first time, we achieve single-crystalline HHB-Cu(Ni) NSs featured with a thickness of 4-5 nm (~8-10 layers) and a lateral size of 0.25-0.65 μm2, as well as single-crystalline HHTP-Cu NSs with a thickness of ~5.1±2.6 nm (~10 layers) and a lateral size of 0.002-0.02 μm2. Benefiting from the ultrathin feature, the synthetic NSs allow fast ion diffusion and high utilization of active sites. As a proof of concept, when serving as a cathode material for Li-ion storage, HHB-Cu NSs deliver a remarkable rate capability (charge within 3 min) and long-term cycling stability (90% capacity retention after 1000 cycles), superior to the corresponding bulk materials and other reported MOF cathodes.
关键词： Li-ion batteries,Two-dimensional conjugated metal-organic frameworks,electrochemical performance,surfactant-assisted synthesis,ultrathin nanosheets
更新于2025-09-23 15:19:57
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Controlled Engineering Nano-sized FeOOH@ZnO Hetero-Structures on Reduced Graphene Oxide for Lithium ion Storage and Photo-Fenton Reaction
摘要： In this work, a nano-sized goethite and zinc oxide hetero-structure (FeOOH@ZnO) dispersed on reduced graphene oxide (RGO) sheets to construct a ternary composite (FeOOH@ZnO/RGO) is first synthesized by a stepped graphene oxide (GO) deoxygenation process. Ferrous ion (Fe2+) and metal Zn were employed as reducing agents, which were transformed to corresponding FeOOH and ZnO nanoparticles to form a hetero-structure in the reaction. Particularly, the size of the nanoparticles can be controlled by limiting the growth kinetics in this work. As a result, porous RGO architecture is constructed with well-dispersed hetero-structured nanoparticles constituted by FeOOH and ZnO nano-crystals encapsulated. The FeOOH@ZnO/RGO composite exhibits unique lithium ion storage properties as anode for lithium ion batteries. And compared with the binary FeOOH/RGO and ZnO/RGO composites, the ternary FeOOH@ZnO/RGO composite shows the best battery performance as anode for lithium ion batteries and the best photo-Fenton degradation activity toward methylene blue (MB) degradation under simulated sunlight irradiation. The preparation route for FeOOH@ZnO/RGO composite is straightforward, effective and has great potential to be scaled-up.
关键词： zinc oxide,goethite,graphene,methylene blue degradation,photo-Fenton,lithium ion batteries
更新于2025-09-23 15:19:57