scholarly journals Upscaling of LATP synthesis: Stoichiometric screening of phase purity and microstructure to ionic conductivity maps

Ionics ◽  
2021 ◽  
Vol 27 (5) ◽  
pp. 2017-2025
Author(s):  
Nikolas Schiffmann ◽  
Ethel C. Bucharsky ◽  
Karl G. Schell ◽  
Charlotte A. Fritsch ◽  
Michael Knapp ◽  
...  

AbstractLithium aluminum titanium phosphate (LATP) is known to have a high Li-ion conductivity and is therefore a potential candidate as a solid electrolyte. Via sol-gel route, it is already possible to prepare the material at laboratory scale in high purity and with a maximum Li-ion conductivity in the order of 1·10−3 s/cm at room temperature. However, for potential use in a commercial, battery-cell upscaling of the synthesis is required. As a first step towards this goal, we investigated whether the sol-gel route is tolerant against possible deviations in the concentration of the precursors. In order to establish a possible process window for sintering, the temperature interval from 800 °C to 1100 °C and holding times of 10 to 480 min were evaluated. The resulting phase compositions and crystal structures were examined by X-ray diffraction. Impedance spectroscopy was performed to determine the electrical properties. The microstructure of sintered pellets was analyzed by scanning electron microscopy and correlated to both density and ionic conductivity. It is shown that the initial concentration of the precursors strongly influences the formation of secondary phases like AlPO4 and LiTiOPO4, which in turn have an influence on ionic conductivity, densification behavior, and microstructure evolution.

2007 ◽  
Vol 336-338 ◽  
pp. 1914-1917
Author(s):  
Lei Yang ◽  
Zhen Yi Zhang ◽  
Xiao Shan Ning ◽  
Guang He Li

In this paper, a novel and highly efficient hydroxyapatite (HA) carrier for cultivating hydrocarbon degradation bacteria (HDB) is introduced. The HA particles synthesized through a sol-gel method and different heat treatments were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and BET method. The microbial amount and activities of HDB cultivated on HA carriers were quantitatively investigated in order to assess their enriching capabilities. The results showed that HA synthesized at 550°C and the one without calcination could enrich HDB 3 and 2 magnitude orders more than the activated carbon, respectively. Mechanisms of bacterial enrichment on HA and activated carbon were also studied, and it is believed that the high bioactivity and the surface morphology of HA were responsible for the efficient reproduction of HDB. It is concluded that HA is a potential candidate to replace the conventionally used activated carbon as a novel carrier applied in the filed of bioremediation for oil contaminated soil.


2008 ◽  
Vol 1122 ◽  
Author(s):  
Gianguido Baldinozzi ◽  
David Simeone ◽  
Dominique Gosset ◽  
Mickael Dollé ◽  
Georgette Petot-Ervas

AbstractWe have synthesized Gd-doped ceria polycrystalline samples (5, 10, 15 %mol), having relative densities exceeding 95% and grain sizes between 30 and 160 nm after axial hot pressing (750 °C, 250 MPa). The samples were prepared by sintering nanopowders obtained by sol-gel chemistry methods having a very narrow size distribution centered at about 16 nm. SEM and X-ray diffraction were performed to characterize the sample microstructures and to assess their structures. We report ionic conductivity measurements using impedance spectroscopy. It is important to investigate the properties of these systems with sub-micrometric grains and as a function of their composition. Therefore, samples having micrometric and nanometric grain sizes (and different Gd content) were studied. Evidence of Gd segregation near the grain boundaries is given and the impact on the ionic conductivity, as a function of the grain size and Gd composition, is discussed and compared to microcrystalline samples.


2015 ◽  
Vol 3 (42) ◽  
pp. 21343-21350 ◽  
Author(s):  
Stefan Breuer ◽  
Denise Prutsch ◽  
Qianli Ma ◽  
Viktor Epp ◽  
Florian Preishuber-Pflügl ◽  
...  

Impedance spectroscopy measurements down to very low temperatures allowed for resolving bulk ion transport properties in highly conducting ceramic electrolytes.


2020 ◽  
Vol 8 (39) ◽  
pp. 20687-20697
Author(s):  
Laura M. de Kort ◽  
Justine Harmel ◽  
Petra E. de Jongh ◽  
Peter Ngene

Tuning the ionic conductivity of LiBH4–LiNH2/oxide nanocomposites by controlling the surface chemistry as well as the porosity of the metal oxide nanoscaffold materials.


2013 ◽  
Vol 1496 ◽  
Author(s):  
Sumaletha Narayanan ◽  
Lina Truong ◽  
Venkataraman Thangadurai

ABSTRACTGarnet-type electrolytes are currently receiving much attention for applications in Li-ion batteries, as they possess high ionic conductivity and chemical stability. Doping the garnet structure has proved to be a good way to improve the Li ion conductivity and stability. The present study includes effects of Y- doping in Li5La3Nb2O12 on Li ion conductivity and stability of “Li5+2xLa3Nb2-xYxO12” (0.05 ≤ x ≤ 0.75) under various environments, as well as chemical stability studies of Li5+xBaxLa3-xM2O12 (M = Nb, Ta) in water. “Li6.5La3Nb1.25Y0.75O12” showed a very high ionic conductivity of 2.7 х 10−4 Scm−1 at 25 °C, which is comparable to the highest value reported for garnet-type compounds, e.g., Li7La3Zr2O12. The selected members show very good stability against high temperatures, water, Li battery cathode Li2CoMn3O8 and carbon. The Li5+xBaxLa3-xNb2O12 garnets have shown to readily undergo an ion-exchange (proton) reaction under water treatment at room temperature; however, the Ta-based garnet appears to exhibit considerably higher stability under the same conditions.


2002 ◽  
Vol 755 ◽  
Author(s):  
Hanxing Liu ◽  
Chen Hu ◽  
Junlei Xia ◽  
Shixi Zhao ◽  
Shixi Ouyang

ABSTRACTIn present study LiMn2O4-xFxwere prepared by the sol-gel method. X-ray diffraction (XRD) and scanning electron microscope (SEM ) were employed to detect the microstructure of the reaction products. It were found perfect crystal particles were obtained, and its' size were uniform in 1∼2 μ m. The specific capacity and cycleability were measured basing on battery program control test system. The results shown the substitution of F for O increased the specific capacity of the material at the cost of the cycleability due to more Mn3+and less Mn4+existed in the material. The exist of Mn3+would reduce cycleability of cathode material due to the Jahn-Teller effect which were caused by the deformation of the crystal structure.


1999 ◽  
Vol 119 (1-4) ◽  
pp. 159-164 ◽  
Author(s):  
M.J.G. Jak ◽  
E.M. Kelder ◽  
Z.A. Kaszkur ◽  
J. Pielaszek ◽  
J. Schoonman

Author(s):  
Martin Reichardt ◽  
Sébastien Sallard ◽  
Petr Novák ◽  
Claire Villevieille

Lithium chromium pyrophosphate (LiCrP2O7) and carbon-coated LiCrP2O7 (LiCrP2O7/C) were synthesized by solid-state and sol–gel routes, respectively. The materials were characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and conductivity measurements. LiCrP2O7 powder has a conductivity of ∼ 10−8 S cm−1, ∼ 104 times smaller than LiCrP2O7/C (∼ 10−4 S cm−1). LiCrP2O7/C is electrochemically active, mainly between 1.8 and 2.2 V versus Li+/Li (Cr3+/Cr2+ redox couple), whereas LiCrP2O7 has limited electrochemical activity. LiCrP2O7/C delivers a reversible specific charge up to ∼ 105 mAh g−1 after 100 cycles, close to the theoretical limit of 115 mAh g−1. Operando XRD experiments show slight peak shifts between 2.2 and 4.8 V versus Li+/Li, and a reversible amorphization between 1.8 and 2.2 V versus Li+/Li, suggesting an insertion reaction mechanism.


Author(s):  
Seonggyu Cho ◽  
Shinho Kim ◽  
Wonho Kim ◽  
Seok Kim ◽  
Sungsook Ahn

Considering the safety issues of Li ion batteries, all-solid-state polymer electrolyte has been one of the promising solutions. In this point, achieving a Li ion conductivity in the solid state electrolytes comparable to liquid electrolytes (>1 mS/cm) is particularly challenging. Employment of polyethylene oxide (PEO) solid electrolyte has not been not enough in this point due to high crystallinity. In this study, hybrid solid electrolyte (HSE) systems are designed with Li1.3Al0.3Ti0.7(PO4)3(LATP), PEO and Lithium hexafluorophosphate (LiPF6) or Lithium bis(trifluoromethanesulfonyl)imide (LiTFSI). Hybrid solid cathode (HSC) is also designed using LATP, PEO and lithium cobalt oxide (LiCoO2, LCO)—lithium manganese oxide (LiMn2O4, LMO). The designed HSE system displays 3.0 × 10−4 S/cm (55 ℃) and 1.8 × 10−3 S/cm (23 ℃) with an electrochemical stability as of 6.0 V without any separation layer introduction. Li metal (anode)/HSE/HSC cell in this study displays initial charge capacity as of 123.4/102.7 mAh/g (55 ℃) and 73/57 mAh/g (25 °C). To these systems, Succinonitrile (SN) has been incorporated as a plasticizer for practical secondary Li ion battery system development to enhance ionic conductivity. The incorporated SN effectively increases the ionic conductivity without any leakage and short-circuits even under broken cell condition. The developed system also overcomes the typical disadvantages of internal resistance induced by Ti ion reduction. In this study, optimized ionic conductivity and low internal resistance inside the Li ion battery cell have been obtained, which suggests a new possibility in the secondary Li ion battery development.


Membranes ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 109 ◽  
Author(s):  
Jadra Mosa ◽  
Jonh Fredy Vélez ◽  
Mario Aparicio

Organic/inorganic hybrid membranes that are based on GTT (GPTMS-TMES-TPTE) system while using 3-Glycidoxypropyl-trimethoxysilane (GPTMS), Trimethyletoxisilane (TMES), and Trimethylolpropane triglycidyl ether (TPTE) as precursors have been obtained while using a combination of organic polymerization and sol-gel synthesis to be used as electrolytes in Li-ion batteries. Self-supported materials and thin-films solid hybrid electrolytes that were doped with Lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) were prepared. The hybrid network is based on highly cross-linked structures with high ionic conductivity. The dependency of the crosslinked hybrid structure and polymerization grade on ionic conductivity is studied. Ionic conductivity depends on triepoxy precursor (TPTE) and the accessibility of Li ions in the organic network, reaching a maximum ionic conductivity of 1.3 × 10−4 and 1.4 × 10−3 S cm−1 at room temperature and 60 °C, respectively. A wide electrochemical stability window in the range of 1.5–5 V facilitates its use as solid electrolytes in next-generation of Li-ion batteries.


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