High Temperature Sintering Research Articles

Mechanical properties and tensile failure behavior of SiCnf/SiC composites with multilayer interphases

SiC fiber-reinforced SiC ceramic matrix composites (SiCf/SiC CMCs) hold potential as thermal structural materials. In this work, SiC nanofibres were coated with multilayer interfaces by magnetron sputtering with the aim to tailor the fiber-matrix interface of SiC nanofibre reinforced SiC composites for superior mechanical properties. The influence of multilayer interface coating and sintering temperature on the density, microstructure, and mechanical properties of SiCnf/SiC CMCs fabricated via a hot-press technique employing ultra-long single-crystal SiC nanofibers as reinforcement were investigated. The composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Transmission electron microscopy (TEM), and a universal testing machine. The prepared CMCs were toughened and strengthened by the observed fiber pull-out and bridging. The multilayered SiCnf/SiC CMCs with multiple interface coatings display an identifiable saw-tooth-like pattern in the load-displacement test, suggesting a significant improvement in the toughness of prepared materials through a laminated structure with weaker interface binding brought on by the thicker, denser coating. In comparison to the SiCnf/SiC composites without interface coating, the prepared SiCnf/SiC CMCs with PyC/SiAlC/ZrC interface layers revealed optimum flexural strength (520 ± 28.88 MPa, ↑46.5 %) and fracture toughness (9.95 ± 0.44 MPa m1/2, ↑94.7 %) after an hour of hot pressing at 1800 °C under pressure of 30 MPa. Besides an increase in relative density at high sintering temperatures (1850 °C), further grain coarsening deteriorated mechanical properties.

Effect of sol impregnation and changes in sol pH on mechanical properties of 3D printed alumina ceramics

This paper reports the successful preparation of high-strength 3D-printed alumina ceramic cores using stereolithography (SLA) and vacuum sol impregnation. Zirconia, alumina, and silica sols (ZS, AS and SS) were chosen as impregnating agents for alumina ceramics. The effects of different types of sols, various ratios of alumina sol to silica sol, and different pH values of sols on the mechanical properties of the ceramics were investigated. The flexural strength of the samples increased significantly after silica sol impregnation, reaching a maximum of 63.51 ± 3.67 MPa, which is 2.06 times higher than that of the unimpregnated samples (UN). Silica particles fill the original pores of the ceramics, and after high-temperature sintering, mullite is formed to increase the density and strength of the ceramics. The flexural strength of alumina ceramics decreases and then increases as the percentage of silica sol in the alumina-silica mixed sol increases. The optimal impregnation ratio for the mixed sols was found to be 1:4, which led to a flexural strength of 62.2 ± 2.09 MPa for the alumina ceramics. In addition, the pH of the sol plays a crucial role in maintaining stable sols. The silica sol is more susceptible to gelation as the pH of the sol increases within the range of 3.5–5.5, which can have a negative impact on its impregnation effectiveness. At a pH of 6.5 in the silica sol, the alumina ceramics exhibited the highest flexural strength of 92.57 ± 2.43 MPa, which is 3.01 times higher than the flexural strength of the unimpregnated samples. The research of impregnation process parameters suitable for 3D printing of alumina ceramics aim to enhance the material's strength, offering a novel solution for applications as high-performance components in the energy sector.

Preparation method and industrialization of Ta-based ultra high temperature ceramic Tujia jar tea baking jar materials

The production materials of traditional Tujia jar tea often face problems such as poor high-temperature performance and poor durability. To improve the temperature resistance and durability of tea baking utensils, this study proposes a new type of TaC ultra-high temperature ceramic. TaC ceramics with excellent performance were prepared through powder metallurgy technology, including high-energy ball milling to ensure uniform mixing, followed by compression molding and high-temperature sintering. The test results demonstrated excellent mechanical properties, with a maximum depth of 948.67 nm and a contact depth of 954.45 nm, proving outstanding compressive and wear resistance. The hardness reached 21.4±0.5 Gpa, and the elastic modulus was 397.2±8.7 Gpa, both of which indicate its stability under high loads. In addition, the fracture toughness was 2.8±0.2 Mpa*m1/2. At a high temperature environment of 1000 °C, the oxidation rate constant of TaC ceramics was only 0.183 mg2 *cm−4 *h, which demonstrates its excellent high-temperature stability. The development of this TaC ceramic not only strengthened the traditional production process of Tujia teapots and tea roasting teapots, thereby improving the product’s service life, but also holds potential for other industrial applications that demand ultra-high temperature stability. These contributions provide new directions for the high-temperature application of ceramic materials and bring tangible economic and technological value to related industries.

Characterization of LiNi0.8Co0.15Al0.05O2 cathode material synthesized via co-precipitation method

Abstract LiNi0.8Co0.15Al0.05O2 cathode material was synthesized using the co-precipitation method, and the effect of synthesis conditions on powder properties was studied. The results indicate that adjusting the pH value and complexing agent concentration during the reaction process can effectively control the precipitation process. The obtained hydroxide precursor is petallike, and the morphology of the cathode material powder after high-temperature sintering is well-dispersed spherical particles. The changes in the sintering system can significantly affect the crystallization process and crystal structure of cathode materials. As the sintering temperature increases, the peak rate I (003)/I (104) significantly decreases, while the R value increases. With the prolongation of sintering time, I (003)/I (104) first increases and then decreases, and the R value first decreases and then increases. After sintering at 750°C × 12 h, the cathode material has the highest peak rate and the lowest R value, indicating the lowest degree of cation mixing, higher structural integrity and the highest electrochemical activity at this time.

Effect of cell sintering temperature on the performance of non-noble metal loaded cerium oxide SOEC anodes

Abstract Introducing methane oxidation reaction into the anode of the high-temperature solid oxide electrolysis cell (SOEC) can reduce the power consumption for water electrolysis. Compared to the traditional conditions of methane oxidation, the methane oxidation catalyst sintered at the SOEC anode, which is closely related to the cell sintering process. This study uses non-noble metals as active sites for methane oxidation, zirconia, and samarium oxides doped ceria as catalyst support and oxygen ion conductors. The effects of anode sintering temperature on the electrochemical performance of SOEC assisted by methane oxidation were investigated. The results indicate that the high-temperature sintering process promotes the performance of the SOEC anode with Ni as the active site, while high temperature harms the performance of the Co-loaded anode. The sintering temperature exhibits a poor effect on the Fe-loaded anode. The Ni exhibits good enhancement of methane oxidation on reducing the electrolysis voltage of SOEC, while Co only exhibits methane oxidation assistance at low-temperature sintering. Differently, Fe has almost no obvious methane oxidation assistance for SOEC, which mainly represents good oxygen evolution performance.

Low-cost iron (Fe) hollow fiber membrane for hydrogen separation

Dense metal membranes are widely studied due to their promising performance in hydrogen separation. In this work, the low-cost dense iron (Fe) hollow fiber membranes (FeHFMs) were developed via the phase inversion and high-temperature sintering method. By tuning the preparation conditions, two typical gas-tight hollow fibers referred to as the sandwich- and honeycomb-structured membranes were successfully synthesized. H2 permeation behavior was well described by Sieverts equation based on the solution-diffusion mechanism. The sandwich-structured FeHFMs had an H2 flux of up to 7.51 mmol m−2 s−1 when operated at a temperature of 850 °C. In comparison, the honeycomb-structured FeHFMs further enhanced the H2 flux by a factor of 3.2 due to the optimized membrane morphology with only one single dense iron layer. The developed FeHFMs showed superior H2 permeation stability in thermal shock tests (40 h) and long-term stability tests (120 h). This work also expanded the potential application horizons of the FeHFMs, which can be easily tailored into porous or dense structures by tuning the sintering conditions.

Ultrafast high-temperature sintering of potassium-sodium niobate: Processing and properties

Current regulations pushing for lead-free piezoelectric alternatives have highlighted potassium-sodium niobate (K0.5Na0.5NbO3, KNN) as a promising candidate. However, conventional sintering of KNN faces challenges like alkali element volatilization and inadequate densification. Ultrafast high-temperature sintering (UHS) offers a solution by rapidly heating ceramics, yielding fine microstructures, with minimal volatile element loss. Here, using a custom UHS equipment we produced undoped KNN ceramics, identifying optimal sintering conditions via a UHS processing map. UHS KNN ceramics sintered for ≤90 s achieved 91 % density, <2 µm average grain size, and no secondary phases. This study reports also the first dielectric, piezoelectric, and ferroelectric properties of UHS KNN ceramics. Differences between as-UHS and post-annealed ceramics were observed as well, with the latter exhibiting piezoelectric coefficients of ~80pC/N. This research enhances understanding of UHS applications and potential of KNN for lead-free piezoelectric uses.

Enhancing the physical properties of Mo-Cu composites through plasma spheroidized spherical molybdenum powder

ABSTRACT This paper investigates the preparation of spherical molybdenum-copper (Mo-Cu) composites through the utilization of plasma spheroidization1 of molybdenum powder, followed by ‘Carbon thermal pre-reduction + Hydrogen deep reduction2’ processes. The properties of these composites are analyzed. By adjusting the mass ratio of molybdenum to copper and employing mechanical activation during high-temperature sintering, Mo and Cu are dispersed more uniformly, resulting in improved fluidity and a reduced tendency to agglomerate in x% Mo-Cu (x = 20, 40, 60, 80) composites. Experimental results demonstrate that compared to original powder Mo-Cu composites, the prepared spherical Mo-Cu composites exhibit uniform elemental distribution, regular arrangement, and reduced porosity. Among these, the 60% Mo (spherical)-Cu composites show the best dispersion and superior performance. At the optimal sintering temperature of 1250°C, the thermal conductivity of the sintered product increased from 137 Wm−1K−1 to 148 Wm−1K−1, the electrical conductivity increased from 18.9 MS/m to 21.8 MS/m, and the Vickers hardness increased from 177 HV to 209 HV.

Breakthrough in atmospheric plasma spraying of high-density composite electrolytes: Deposition behavior and performance of plasma-sprayed GDC-LSGM on porous metal-supported solid oxide fuel cells

The potential application of plasma spraying in the preparation of ceramic electrolyte for porous metal-supported solid oxide fuel cells (SOFCs) is highlighted by its ability to eliminate the need for a high-temperature sintering process. However, the challenge of achieving highly dense electrolytes through plasma spraying remains to be addressed. In this study, a novel electrolyte for porous metal-supported SOFCs (PMS-SOFCs) is developed. This involved the preparation of a highly dense structure of gadolinium-doped ceria (GDC)-lanthanum strontium gallium magnesium oxide (LSGM) composite coating using plasma spraying under atmospheric conditions. The composite electrolyte is prepared using atmospheric plasma spraying (APS). The addition of the low-melting-point LSGM phase enhanced the microstructural densification of the GDC-based composite coating and diminished electron loss in a reducing atmosphere, thereby improving the cell's open-circuit voltage. At 36 kW plasma arc power, the single cell with composite electrolyte exhibited a maximum power density of 371 mw/cm2 at 750 °C and achieved the highest open-circuit voltage (1.03 V) at 600 °C. Moreover, the open-circuit voltage remained stable over a 100-h test. These findings suggest that using APS to deposit a composite electrolyte with added low-melting-point secondary phases presents a promising approach for achieving relatively high OCV in PMS-SOFCs based on cerium oxide electrolytes.

Study on electrical conductive mechanism of mayenite derivative C12A7:C

Abstract This study explains the conductive mechanism of C12A7:C from the perspective of crystal structure. C12A7:C is a carbon derivative of C12A7 and prepared by CaCO3 and Al2O3 in sealed graphite crucible through high-temperature sintering experiments. The main component was confirmed to be C12A7:C through X-ray diffraction inversion analysis. The four-probe method revealed that it is a semiconductor with conductivity of 4,339 S/m. A conductive model of C12A7:C crystal was established to study its conductive mechanism. Through theoretical calculations of the conductive structure model, the density of states and transfer function are important factors determining the conductivity of C12A7:C crystals. Based on the analysis of these two factors, C is the key to electron transfer in the C12A7:C crystal. Further research indicates that the C–C bond is the main form of C in C12A7:C crystals. These C–C bonds satisfy the formation conditions of conjugated systems and are key to the conductivity of C12A7:C crystals. Through simulation calculations, the volt ampere characteristic curve of C12A7:C exhibits Ohmic conductor characteristics. The conductivity of C12A7:C obtained through theoretical calculation is consistent with the experimental results. In conclusion, the conductivity of C12A7:C crystal is mainly due to the C–C conjugated system formed by carbon atoms in the crystal.

Lithium Pre-Storage Enables High Initial Coulombic Efficiency and Stable Lithium-Enriched Silicon/Graphite Anode.

Application of silicon-based anodes is significantly challenged by low initial Coulombic efficiency (ICE) and poor cyclability. Traditional pre-lithiation reagents often pose safety concerns due to their unstable chemical nature. Achieving a balance between water-stability and high ICE in prelithiated silicon is a critical issue. Here, we present a lithium-enriched silicon/graphite material with an ultra-high ICE of ≥110 % through a high-stable lithium pre-storage methodology. Lithium pre-storage prepared a nano-drilled graphite material with surficial lithium functional groups, which can form chemical bonds with adjacent silicon during high-temperature sintering. This results in an unexpected O-Li-Si interaction, leading to in situ pre-lithiation of silicon nanoparticles and providing high stability in air and water. Additionally, the lithium-enriched silicon/graphite materials impart a combination of high ICE, high specific capacity (620 mAh g-1), and long cycling stability (>400 cycles). This study opens up a promising avenue for highly air- and water-stable silicon anode prelithiation methods.

The Crystal Structure of Al4SiC4 Revisited.

Al4SiC4 is a ternary wide-band-gap semiconductor with a high strength-to-weight ratio and excellent oxidation resistance. It consists of slabs of Al4C3 separated by SiC layers with the space group of P63mc. The space group allows Si to occupy two different 2a Wykoff sites, with previous studies reporting that Si occupies only one of the two sites, giving it an ordered structure. Another hitherto unexplored possibility is that Si can be randomly distributed on both 2a sites. In this work, we revisit the published ordered crystal structure using experimental methods and density functional theory (DFT). Al4SiC4 was synthesized by high-temperature sintering at 1800 °C from a powder mixture of Al4C3 and SiC. Neutron diffraction confirmed that Al4SiC4 crystallized with the space group of P63mc, with diffraction patterns that could be fitted to both the ordered and the disordered structures. Scanning transmission electron microscopy, however, provided clear evidence supporting the latter, with DFT calculations further confirming that it is 0.16 eV lower in energy per Al4SiC4 formula unit than the former. TEM analysis revealed Al vacancies in some of the atomic layers that can introduce p-type doping and direct band gaps of 0.7 and 1.2 eV, agreeing with our optical measurements. Finally, we propose that although the calculated formation energy of the Al vacancies is high, the vacancies are stabilized by entropy effects at the high synthesis temperature. This indicates that the cooling procedure after high-temperature synthesis can be important in determining the vacancy content and the electronic properties of Al4SiC4.

Low-temperature properties of magnetically frustrated rare-earth zirconates A 2Zr2O7

Rare-earth A 2Zr2O7 zirconates have attracted considerable attention of the scientific community for their complex magnetic, electronic and material properties applicable in modern technologies. The light rare-earth members of the series, crystallising in the pyrochlore variant of cubic crystal structure, have been studied in detail. The heavier A 2Zr2O7 compounds have been investigated mainly from the material properties viewpoint, focussing on their thermal properties and stability at high temperature and pressure. Low-temperature studies were mostly missing until recently. We present the low-temperature magnetic and thermodynamic properties of A 2Zr2O7 with A = Y, La, Nd, Eu, Gd, Tb, Dy, Ho, Tm, Yb, and Lu, well covering the whole series, newly synthesised by high-temperature sintering and melting methods. X-ray diffraction reveals and confirms the ordered pyrochlore structure in the light members, the disordered cubic structure of the defect-fluorite type in A 2Zr2O7 with A = Y, Gd–Yb, and finally the lower symmetry rhombohedral structure in the end-member Lu2Zr2O7. The specific heat of the investigated compounds is dominated by a low-temperature anomaly associated with magnetic ordering: long-range in light rare-earth zirconates; and short-range in heavier members. The effective magnetic moment in the studied compounds, determined by fitting the magnetisation data to the Curie–Weiss formula, is in good agreement with the expected value of the A 3+ free ion. The magnetic properties have been revealed to be strongly influenced by the geometric frustration of the magnetic moments of both the pyrochlore structure, as well as the face centred cubic lattice created by the cations of the defect-fluorite structure, but connected also to intrinsic atomic disorder. The experimental results are discussed in the framework of previous studies on A 2Zr2O7 zirconates, as well as other A 2 B 2O7 compounds.

Preparation of egg-structured ceramsites from molybdenum tailings with improved properties

Conversion of solid waste tailings into building materials is an effective way to turn waste into resources as well as resolve the problems of their accumulation and pollution. Herein, in this paper, light-weight and high strength molybdenum tailings ceramsites (LHMCs) were prepared using molybdenum tailings as the main raw material supplemented with fly ash, sludge, steel slag and other solid wastes by egg-structure (three-layer structure) design and high-temperature sintering. The effects of raw material ratio, amount of carbon powder agent, sintering temperature, and sintering time on the properties of LHMCs were investigated, and the optimal preparation process was proposed to be preheating at 400 °C for 60 min and sintering at 1150 °C for 40 min. The results of the physicochemical properties, morphology, and component analysis of LHMCs show that the LHMCs with egg-structure including porous core, reinforced middle layer, and dense outer layer can significantly increase the strength of the ceramsites under the premise of ensuring the low density of the ceramsites. Meanwhile, the doping of molybdenum tailings improves the physical properties of the ceramsites and achieves the reuse of waste tailings. Importantly, the optimized LHMCs can meet the performance requirements of 900-grade ceramsites. This paper proposes a strategy for the preparation of tailings-doped light-weight and high-strength ceramic building materials, which provides a new idea for the recycling of solid waste.

Reasonable design a high-entropy garnet-type solid electrolyte for all-solid-state lithium batteries

Traditional garnet solid electrolyte (Li7La3Zr2O12) suffers from low room temperature ionic conductivity, poor air stability, high sintering temperature and energy consumption. Considering the development prospects of high-entropy materials with high structural disorder and strong component controllability in the field of electrochemical energy storage, herein, a novel high-entropy garnet-type oxide solid electrolyte, Li5.75Ga0.25La3Zr0.5Ti0.5Sn0.5Nb0.5O12 (LGLZTSNO) was constructed by partially replacing the Li and Zr sites in Li7La3Zr2O12 with Ga and Ti/Sn/Nb elements, respectively. The experimental and density functional theory (DFT) calculation results show that the high-entropy LGLZTSNO electrolyte has preferable room temperature ion conductivity, air stability, interface contact performance with lithium anode, and the ability to suppress lithium dendrites. Thanks to the improvement of electrolyte performance, the critical current density of Li/Ag@LGLZTSNO/Li symmetric cell was increased from 0.42 to 1.57 mA cm−2, and the interface area specific impedance (IASR) was reduced from 765.2 to 42.3 Ω cm2. Meanwhile, the Li/Ag@LGLZTSNO/LFP full cell also exhibits excellent rate performance and cycling performance (148 mA h g−1 at 0.1 C and 124 mA h g−1 at 0.5 C, capacity retention up to 84.8% after 100 cycles at 0.1 C), showing the application prospects of high-entropy LGLZTSNO solid electrolyte in high-performance all solid state lithium batteries.

Effect of nitrogen addition on sintering behavior of high-entropy alloy CrMnFeCoNi powder

The effect of nitrogen addition on sintering behavior of high-entropy alloy CrMnFeCoNi powder has been investigated. CrMnFeCoNi alloy powders were nitrided to add nitrogen and then consolidated at three different temperatures. The microstructure of the nitrided CrMnFeCoNi alloy powders and sintered compacts was characterized using electron probe microanalysis (EPMA) system. In the compact sintered at 800 °C, a high-nitrogen-content region formed a continuous network structure around the low-nitrogen-content substrate. The hardness of the sintered compacts with nitrogen was higher than that of the compacts without nitrogen. The high-nitrogen-content region expanded into the substrate region. The Vickers hardness of the sintered compacts increased with an increase of sintering temperature up to 950 °C. Sintering at 1100 °C did not completely finish; the vacuum pressure in the sintering chamber rapidly increased because chromium nitride (CrN) decomposed. The results indicate that high-temperature sintering is ineffective for nitrogen-added CrMnFeCoNi alloy powder.

Boron-incorporated IrO2-Ta2O5 coating as an efficient electrocatalyst for acidic oxygen evolution reaction

The Ir-based electrocatalysts for the acidic oxygen evolution reaction (OER) have demonstrated remarkable durability. Enhancing the Ir-based electrocatalytic activity still remains crucial owing to the scarcity of iridium. Here, a high-temperature sintering technique is employed to fabricate a boron (B)-incorporated IrO2-Ta2O5 coating with an almost perfect rutile-type crystal structure on a corrosion-resistant titanium substrate, ensuring exceptional stability for the acidic OER. The B-incorporated IrO2-Ta2O5 electrode fabricated in a mixed solution of 0.6 M H3BO3, exhibits an overpotential of 210 mV at a current density of 10 mA cm−2 and a lower Tafel slope of 34.2 mV dec−1 in a 0.5 M H2SO4 solution, which is far lower than the 272 mV overpotential and the 45.3 mV dec−1 of the IrO2-Ta2O5/Ti electrode. The electrode possesses a minimal potential increase even after undergoing continuous OER for 400 h at a high current density of 100 mA cm−2 in a 0.5 M H2SO4 solution. The incorporation of B species into IrO2-Ta2O5 effectively fine-tunes the electronic structure of Ir active sites, leading to a substantial enhancement of the intrinsic electrocatalytic activity. This study provides promising prospects for reducing the energy consumption of noble IrO2-based electrocatalysts in the practical application of electrochemical industry for the acidic OER.

Innovations in Electric Current-Assisted Sintering for SOFC: A Review of Advances in Flash Sintering and Ultrafast High-Temperature Sintering

This review discusses the groundbreaking advancements in electric current-assisted sintering techniques, specifically Flash Sintering (FS) and Ultrafast High-Temperature Sintering (UHS), for their application in Solid Oxide Fuel Cells (SOFCs). These innovative sintering methods have demonstrated remarkable potential in enhancing the efficiency and quality of SOFC manufacturing by significantly lowering sintering temperatures and durations, thereby mitigating energy consumption and cost. By providing a detailed overview of the mechanisms, process parameters, and material characteristics associated with FS and UHS, this paper sheds light on their pivotal role in the fabrication of SOFC components such as electrolytes, electrodes, multilayered materials, and interconnect coatings. The advantages, challenges, and prospective opportunities of these sintering technologies in propelling SOFC advancements are thoroughly assessed, underlining their transformative impact on the future of clean and efficient energy production technologies.

Evaluation of the Combustion Properties and Catalytic Activity of MgAlB Energetic Ternary Particles

ABSTRACT Boron powder possesses significant potential for use as a combustible agent in energetic materials, owing to its superior combustion thermodynamic properties. However, the powder’s tendency to form an oxide layer on its surface results in delayed ignition, reduced combustion efficiency, and compromised energy advantage. To enhance the ignition and combustion properties of boron powder, we prepared boron-based energetic composites containing flammable metals (MgxAl1-xB2) through high-temperature sintering. These were then characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), energy dispersive spectroscopy (EDS). The combustion heat of these alloy powders were measured using an oxygen bomb calorimeter, while their catalytic performance on the thermal decomposition of ammonium perchlorate (AP) was analyzed using differential scanning calorimetry (DSC) and differential thermal analysis (DTA). The results indicate that compared with boron, the MgxAl1-xB2 powders are more flammable, require less oxygen, exhibit a higher combustion efficiency and exothermic advantage. Especially, the Mg0.9Al0.1B2 and MgB2 alloy exhibit optimal combustion heat values of 39,094.92 and 37,693.90 J·g−1, respectively. They significantly enhance the thermal decomposition of AP and reduce the activation energy by over 20%.

Na3MnTi(PO4)3/C Nanofiber Free-Standing Electrode for Long-Cycling-Life Sodium-Ion Batteries.

Self-standing Na3MnTi(PO4)3/carbon nanofiber (CNF) electrodes are successfully synthesized by electrospinning. A pre-synthesized Na3MnTi(PO4)3 is dispersed in a polymeric solution, and the electrospun product is heat-treated at 750 °C in nitrogen flow to obtain active material/CNF electrodes. The active material loading is 10 wt%. SEM, TEM, and EDS analyses demonstrate that the Na3MnTi(PO4)3 particles are homogeneously spread into and within CNFs. The loaded Na3MnTi(PO4)3 displays the NASICON structure; compared to the pre-synthesized material, the higher sintering temperature (750 °C) used to obtain conductive CNFs leads to cell shrinkage along the a axis. The electrochemical performances are appealing compared to a tape-casted electrode appositely prepared. The self-standing electrode displays an initial discharge capacity of 124.38 mAh/g at 0.05C, completely recovered after cycling at an increasing C-rate and a coulombic efficiency ≥98%. The capacity value at 20C is 77.60 mAh/g, and the self-standing electrode exhibits good cycling performance and a capacity retention of 59.6% after 1000 cycles at 1C. Specific capacities of 33.6, 22.6, and 17.3 mAh/g are obtained by further cycling at 5C, 10C, and 20C, and the initial capacity is completely recovered after 1350 cycles. The promising capacity values and cycling performance are due to the easy electrolyte diffusion and contact with the active material, offered by the porous nature of non-woven nanofibers.