Volume 15 Issue 1, July 2025
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Structural and Thermal Characterisation of Lithium Aluminium Titanium Tantalum Phosphate NASICON-type Solid Electrolyte
The material with NASICON-type structure lithium aluminium titanium phosphate with tantalum substituting titanium Li1.3Al0.3Ti1.66Ta0.04(PO4)3 (LATTaP) has been synthesised via the solid-state method at a sintering temperature of 900 ºC for 6 h. The thermal analysis indicated that the reaction of the chemical mixture becomes stable around 717 ºC, indicating an improvement in the material densification. FTIR shows the presence of NASICON phosphate peaks, which were dominated by the vibration of the PO4 ionic group. This also confirms the presence of LiTi2(PO4)3 in all of the samples. The X-ray powder diffraction analysis shows the effect of tantalum in the composition LATTaP. The single phase has been observed due to tantalum substitution with a total conductivity of σ = 1.35 x 10-4 S/cm. These findings suggest that the composition has the potential to be used as a solid electrolyte material in lithium-ion rechargeable batteries. This material will contribute to better NASICON material for solid electrolytes.
Authors: *1,2 Sanda Abubakar Sadiq, 2Mohammed Isah Kimpa, 2Ibrahim Sharifat Olalonpe, and 2Isah Kasim Uthman 1 Department of Physics, Faculty of Natural Science, Ibrahim Badamasi Babangida University Lapai, P.M.B 11 Lapai, Niger State, Nigeria. 2 Department of Physics, School of Physical Sciences, Federal University of Technology Minna, P.M.B 65 Minna, Niger State, Nigeria.
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Abstract
The material with NASICON-type structure lithium aluminium titanium phosphate with tantalum substituting titanium Li1.3Al0.3Ti1.66Ta0.04(PO4)3 (LATTaP) has been synthesised via the solid-state method at a sintering temperature of 900 ºC for 6 h. The thermal analysis indicated that the reaction of the chemical mixture becomes stable around 717 ºC, indicating an improvement in the material densification. FTIR shows the presence of NASICON phosphate peaks, which were dominated by the vibration of the PO4 ionic group. This also confirms the presence of LiTi2(PO4)3 in all of the samples. The X-ray powder diffraction analysis shows the effect of tantalum in the composition LATTaP. The single phase has been observed due to tantalum substitution with a total conductivity of σ = 1.35 x 10-4 S/cm. These findings suggest that the composition has the potential to be used as a solid electrolyte material in lithium-ion rechargeable batteries. This material will contribute to better NASICON material for solid electrolytes.
Advances in Sol-Gel Synthesis of MgZr4(1-x)Hf4xP6O24 (x = 0, 1) Solid Electrolytes for Electrochemical Devices
The potential solid electrolytes, MgZr4P6O24 and MgHf4P6O24 were prepared using modified novel sol-gel method. Structural and electrical properties of the solid electrolytes were determined. TGA-DSC analyses indicated that the pure dried xerogel powders, when calcined at 900 oC converts to pure single phase MgZr4P6O24 and MgHf4P6O24 nanopowders with excellent crystallinity. Pellets of 13 mm diameter and 3.8 mm thickness made by uniaxial compression were respectively sintered at 1300 oC. Powder XRD analyses indicated that crystalline phase of MgZr4P6O24 and MgHf4P6O24 nanoparticles exhibit monoclinic structure with crystallite size of approx. 39 mm and 42 mm, respectively. The sintered pellets were stable from 1000 oC to 1300 oC, with MgHf4P6O24 solid electrolyte showing no trace of coexistent second phase at higher temperatures. Relative density analyses of sintered MgZr4P6O24 and MgHf4P6O24 pellets yield optimum density of approx. 99% and 98% at 1300 oC, respectively, which are in perfect agreement with SEM-EDS analyses of the sintered pellets. Using impedance spectroscopy, the bulk ionic conductivity of the platinum-cured sintered MgZr4P6O24 and MgHf4P6O24 pellets were determined as 7.23 x 10-3 Scm-1 at 725 oC and 4.52 x 10-4 Scm-1 at 747 oC, respectively. Activation energy of MgZr4P6O24 (Ea = 0.84±0.04eV) and gHf4P6O24 (Ea = 0.74±0.02eV) solid electrolytes indicating MgZr4P6O24 solid electrolyte as possessing improved Mg2+-ion conducting mobile species at high temperatures. However, both solid electrolytes find suitable applications in electrochemical devices.
Authors: Mohammed Alhaji Adamu, Girish M Kale
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Abstract
The potential solid electrolytes, MgZr4P6O24 and MgHf4P6O24 were prepared using modified novel sol-gel method. Structural and electrical properties of the solid electrolytes were determined. TGA-DSC analyses indicated that the pure dried xerogel powders, when calcined at 900 oC converts to pure single phase MgZr4P6O24 and MgHf4P6O24 nanopowders with excellent crystallinity. Pellets of 13 mm diameter and 3.8 mm thickness made by uniaxial compression were respectively sintered at 1300 oC. Powder XRD analyses indicated that crystalline phase of MgZr4P6O24 and MgHf4P6O24 nanoparticles exhibit monoclinic structure with crystallite size of approx. 39 mm and 42 mm, respectively. The sintered pellets were stable from 1000 oC to 1300 oC, with MgHf4P6O24 solid electrolyte showing no trace of coexistent second phase at higher temperatures. Relative density analyses of sintered MgZr4P6O24 and MgHf4P6O24 pellets yield optimum density of approx. 99% and 98% at 1300 oC, respectively, which are in perfect agreement with SEM-EDS analyses of the sintered pellets. Using impedance spectroscopy, the bulk ionic conductivity of the platinum-cured sintered MgZr4P6O24 and MgHf4P6O24 pellets were determined as 7.23 x 10-3 Scm-1 at 725 oC and 4.52 x 10-4 Scm-1 at 747 oC, respectively. Activation energy of MgZr4P6O24 (Ea = 0.84±0.04eV) and gHf4P6O24 (Ea = 0.74±0.02eV) solid electrolytes indicating MgZr4P6O24 solid electrolyte as possessing improved Mg2+-ion conducting mobile species at high temperatures. However, both solid electrolytes find suitable applications in electrochemical devices.