Influence of LiBF4 sintering aid on the microstructure and conductivity of LATP solid electrolyte

Dai, Lijing; Wang, Jing; Shi, Zhang; Yu, Lina; Shi, Jun

doi:10.1016/j.ceramint.2021.01.004

Cited by 54 publications

(39 citation statements)

References 15 publications

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“…800 • C, we observed the formation of the LiTiPO 5 compound, which was not present in the base LATP material. 31 P MAS NMR results also confirmed the presence of this compound in the composite material. Besides the formation of the LiTiPO 5 phase, MAS NMR data reveal the presence of additional resonances ascribed to Li 4 P 2 O 7 and LiAlP 2 O 7 compounds, and also to another unidentified phase.…”

Section: Discussionsupporting

confidence: 56%

“…Considering 29 Si MAS NMR spectra and XRD results, we conclude that the Li 4 SiO 4 additive material decomposed into Li 2 O and SiO 2 . In parallel, 31 P MAS NMR spectra also showed the incorporation of additional Al 3+ ions into NASICON grains, substituting Ti 4+ ions. However, to perform such substitution, lithium ions should also diffuse into the grains of LATP.…”

Section: Mas Nmrmentioning

confidence: 88%

“…The impedance data was collected using a self-developed software [36]. 27 Al, 6 Li, 29 Si, and 31 P MAS NMR spectra were recorded with a Bruker AVANCE-400 spectrometer (9.4T magnetic field) and the resonance frequencies were 104.3, 58.9, 79.5, and 162.0 MHz, respectively. For single-pulse 27 Al and 6 Li MAS NMR spectra, π/6 pulses of 2 µs were used, but for 31 P and 29 Si spectra, 4 µs irradiation (π/2 pulses) were applied.…”

Section: Polycrystallinementioning

confidence: 99%

“…Grain boundary conductivity of LATP was found to be highly dependent on the sintering process, resulting in different particle size distributions (i.e., microstructure) and different impurity phases [8,10,11,14,[23][24][25][26]. The effectiveness of the LATP sintering process can be considerably improved by the use of appropriate sintering agents, such as LiF [14,27,28], Li 3 PO 4 [29], Li 3 BO 3 [24,29], LiBO 2 [30], LiBF 4 [31], LiNO 3 [32], Li 2 O [33], and Li 4 SiO 4 [this work]. These inorganic salts are known to affect the microstructure (lower porosity) and secondary phase formation, leading to higher total ionic conductivity.…”

Section: Introductionmentioning

confidence: 99%

“…Figure5 31. P MAS NMR spectra of LATP-0.1LSO sintered at 900 and 1000 • C for 2, 6, or 12 h. The experimental and simulated spectra are displayed as black and red lines, respectively.…”

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confidence: 99%

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Electrical and Structural Properties of Li1.3Al0.3Ti1.7(PO4)3—Based Ceramics Prepared with the Addition of Li4SiO4

et al. 2021

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The currently studied materials considered as potential candidates to be solid electrolytes for Li-ion batteries usually suffer from low total ionic conductivity. One of them, the NASICON-type ceramic of the chemical formula Li1.3Al0.3Ti1.7(PO4)3, seems to be an appropriate material for the modification of its electrical properties due to its high bulk ionic conductivity of the order of 10−3 S∙cm−1. For this purpose, we propose an approach concerning modifying the grain boundary composition towards the higher conducting one. To achieve this goal, Li4SiO4 was selected and added to the LATP base matrix to support Li+ diffusion between the grains. The properties of the Li1.3Al0.3Ti1.7(PO4)3−xLi4SiO4 (0.02 ≤ x ≤ 0.1) system were studied by means of high-temperature X-ray diffractometry (HTXRD); 6Li, 27Al, 29Si, and 31P magic angle spinning nuclear magnetic resonance spectroscopy (MAS NMR); thermogravimetry (TG); scanning electron microscopy (SEM); and impedance spectroscopy (IS) techniques. Referring to the experimental results, the Li4SiO4 additive material leads to the improvement of the electrical properties and the value of the total ionic conductivity exceeds 10−4 S∙cm−1 in most studied cases. The factors affecting the enhancement of the total ionic conductivity are discussed. The highest value of σtot = 1.4 × 10−4 S∙cm−1 has been obtained for LATP–0.1LSO material sintered at 1000 °C for 6 h.

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Section: Discussionsupporting

confidence: 56%

Section: Mas Nmrmentioning

confidence: 88%

Section: Polycrystallinementioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

“…Figure5 31. P MAS NMR spectra of LATP-0.1LSO sintered at 900 and 1000 • C for 2, 6, or 12 h. The experimental and simulated spectra are displayed as black and red lines, respectively.…”

mentioning

confidence: 99%

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Electrical and Structural Properties of Li1.3Al0.3Ti1.7(PO4)3—Based Ceramics Prepared with the Addition of Li4SiO4

et al. 2021

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Recent Advances in Conduction Mechanisms, Synthesis Methods, and Improvement Strategies for Li₁₊_xAl_xTi₂₋_x(PO₄)₃ Solid Electrolyte for All‐Solid‐State Lithium Batteries

Zhou

et al. 2022

Advanced Energy Materials

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With the increasing use of Li batteries for storage, their safety issues and energy densities are attracting considerable attention. Recently, replacing liquid organic electrolytes with solid‐state electrolytes (SSE) has been hailed as the key to developing safe and high‐energy‐density Li batteries. In particular, Li1+xAlxTi2−x(PO4)3 (LATP) has been identified as a very attractive SSE for Li batteries due to its excellent electrochemical stability, low production costs, and good chemical compatibility. However, interfacial reactions with electrodes and poor thermal stability at high temperatures severely restrict the practical use of LATP in solid‐state batteries (SSB). Herein, a systematic review of recent advances in LATP for SSBs is provided. This review starts with a brief introduction to the development history of LATP and then summarizes its structure, ion transport mechanism, and synthesis methods. Challenges (e.g., intrinsic brittleness, interfacial resistance, and compatibility) and corresponding solutions (ionic substitution, additives, protective layers, composite electrolytes, etc.) that are critical for practical applications are then discussed. Last, an outlook on the future research direction of LATP‐based SSB is provided.

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Interface Welding via Thermal Pulse Sintering to Enable 4.6 V Solid‐State Batteries

Yao,

Chen,

Wang

et al. 2023

Advanced Energy Materials

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NASICON‐type Li1.3Al0.3Ti1.7(PO4)3 (LATP) is one of the most promising solid‐state electrolytes (SSEs) to achieve high‐energy‐density solid‐state batteries (SSBs) due to its high ionic conductivity, high‐voltage stability, and low cost. However, its practical application is constrained by inadequate interfacial compatibility with cathode materials and significant incompatibility with lithium metal. In this work, a cost‐effective interface welding approach is reported, utilizing an innovative thermal pulse sintering (TPS) to fabricate LATP‐based solid‐state batteries. Initially, the rapid thermal pulses enhance the ionic conductivity of LATP SSE by inducing selective growth of LATP nanowires, effectively occupying interparticle voids. Additionally, this process results in the formation of a dense layer (GCM) comprising graphene oxide, carbon nanotubes, and MXene with a controlled Li+ transport pathway, facilitating lithium stripping and plating processes. Moreover, these thermal pulses facilitate the interfacial fusion between LATP and cathode materials, while avoiding undesired phase diffusion. As a result, SSBs with a LiCoO2 cathode deliver favorable cycle stability at 4.6 V, marking significant progress. This facile interface welding strategy represents a substantial step toward high‐energy‐density SSB development.

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Influence of LiBF4 sintering aid on the microstructure and conductivity of LATP solid electrolyte

Cited by 54 publications

References 15 publications

Electrical and Structural Properties of Li1.3Al0.3Ti1.7(PO4)3—Based Ceramics Prepared with the Addition of Li4SiO4

Electrical and Structural Properties of Li1.3Al0.3Ti1.7(PO4)3—Based Ceramics Prepared with the Addition of Li4SiO4

Recent Advances in Conduction Mechanisms, Synthesis Methods, and Improvement Strategies for Li₁₊_xAl_xTi₂₋_x(PO₄)₃ Solid Electrolyte for All‐Solid‐State Lithium Batteries

Interface Welding via Thermal Pulse Sintering to Enable 4.6 V Solid‐State Batteries

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Influence of LiBF4 sintering aid on the microstructure and conductivity of LATP solid electrolyte

Cited by 54 publications

References 15 publications

Electrical and Structural Properties of Li1.3Al0.3Ti1.7(PO4)3—Based Ceramics Prepared with the Addition of Li4SiO4

Electrical and Structural Properties of Li1.3Al0.3Ti1.7(PO4)3—Based Ceramics Prepared with the Addition of Li4SiO4

Recent Advances in Conduction Mechanisms, Synthesis Methods, and Improvement Strategies for Li1+xAlxTi2−x(PO4)3 Solid Electrolyte for All‐Solid‐State Lithium Batteries

Interface Welding via Thermal Pulse Sintering to Enable 4.6 V Solid‐State Batteries

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Recent Advances in Conduction Mechanisms, Synthesis Methods, and Improvement Strategies for Li₁₊_xAl_xTi₂₋_x(PO₄)₃ Solid Electrolyte for All‐Solid‐State Lithium Batteries