Physiochemical characterization and electrochemical impedance spectroscopic analysis of NASICON based M1+xAlxTi2-x (PO4)3 electrolytes for solid state batteries

Zunaira Zulfiqar; Khalid Aljohani; Amna Mir; Rizwan Raza; Michal Mazur; Qaisar Abbas

doi:10.1002/est2.70245

Physiochemical characterization and electrochemical impedance spectroscopic analysis of NASICON based M_1+xAl_xTi_2-x (PO₄)₃ electrolytes for solid state batteries

Zunaira Zulfiqar
, Khalid Aljohani
, Amna Mir
, Rizwan Raza^*
, Michal Mazur
, Qaisar Abbas^*

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

Abstract

The suitability of NASICON-based M_1+xAl_xTi_2−x(PO₄)₃, where M = Li, Na, and x = 0.5 solid-state electrolytes was investigated. Electrolytes were synthesized using high-temperature annealing of NH₄H₂PO₄, TiO₂, and Al₂O₃ compounds followed by ball milling. Synthesized samples displayed a single crystalline phase like NASICON-type material with space group R3c. X-ray photoelectron spectroscopy and Raman spectrum confirmed the absence of impurities in samples, establishing elemental consistency. Microstructure analysis was performed using field emission scanning electron microscopy; samples displayed a granular surface with agglomeration of these grains in a radius of a few micrometers. Electrochemical impedance spectroscopy study showed that the conductivity of samples increased with increasing working temperature, and the highest conductivity values for Li_1.5Al_0.5Ti_1.5(PO₄)₃ and Na_1.5Al _0.5Ti_1.5(PO₄)₃ at 150°C were found to be 3.5 × 10⁻⁴ and 5.3 × 10⁻⁴Scm⁻¹, respectively. Findings reinforce the suitability of these electrolytes, offering a basis for future work in solid batteries in general and for lithium-ion and sodium-ion batteries in particular.

Original language	English
Article number	e70245
Number of pages	12
Journal	Energy Storage
Volume	7
Issue number	5
DOIs	https://doi.org/10.1002/est2.70245
Publication status	Published - 4 Aug 2025

UN SDGs

This output contributes to the following UN Sustainable Development Goals (SDGs)

SDG 7 Affordable and Clean Energy

Keywords

activation energy
diffusion mechanism
electrical conductivities
energy storage
lithium-ion batteries
polyethylene glycol
sodium-ion batteries
solid state electrolytes

Access to Document

10.1002/est2.70245

Embargoed Document

Zulfiqar et al Physiochemical accepted - for Pure
Accepted author manuscript, 757 KB
Embargo ends: 4/08/26

Cite this

@article{3c45139aeaa144d6a916baf2ae108612,

title = "Physiochemical characterization and electrochemical impedance spectroscopic analysis of NASICON based M1+xAlxTi2-x (PO4)3 electrolytes for solid state batteries",

abstract = "The suitability of NASICON-based M1+xAlxTi2−x(PO4)3, where M = Li, Na, and x = 0.5 solid-state electrolytes was investigated. Electrolytes were synthesized using high-temperature annealing of NH4H2PO4, TiO2, and Al2O3 compounds followed by ball milling. Synthesized samples displayed a single crystalline phase like NASICON-type material with space group R3c. X-ray photoelectron spectroscopy and Raman spectrum confirmed the absence of impurities in samples, establishing elemental consistency. Microstructure analysis was performed using field emission scanning electron microscopy; samples displayed a granular surface with agglomeration of these grains in a radius of a few micrometers. Electrochemical impedance spectroscopy study showed that the conductivity of samples increased with increasing working temperature, and the highest conductivity values for Li1.5Al0.5Ti1.5(PO4)3 and Na1.5Al 0.5Ti1.5(PO4)3 at 150°C were found to be 3.5 × 10−4 and 5.3 × 10−4 Scm−1, respectively. Findings reinforce the suitability of these electrolytes, offering a basis for future work in solid batteries in general and for lithium-ion and sodium-ion batteries in particular.",

keywords = "activation energy, diffusion mechanism, electrical conductivities, energy storage, lithium-ion batteries, polyethylene glycol, sodium-ion batteries, solid state electrolytes",

author = "Zunaira Zulfiqar and Khalid Aljohani and Amna Mir and Rizwan Raza and Michal Mazur and Qaisar Abbas",

year = "2025",

month = aug,

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doi = "10.1002/est2.70245",

language = "English",

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issn = "2578-4862",

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T1 - Physiochemical characterization and electrochemical impedance spectroscopic analysis of NASICON based M1+xAlxTi2-x (PO4)3 electrolytes for solid state batteries

AU - Zulfiqar, Zunaira

AU - Aljohani, Khalid

AU - Mir, Amna

AU - Raza, Rizwan

AU - Mazur, Michal

AU - Abbas, Qaisar

PY - 2025/8/4

Y1 - 2025/8/4

N2 - The suitability of NASICON-based M1+xAlxTi2−x(PO4)3, where M = Li, Na, and x = 0.5 solid-state electrolytes was investigated. Electrolytes were synthesized using high-temperature annealing of NH4H2PO4, TiO2, and Al2O3 compounds followed by ball milling. Synthesized samples displayed a single crystalline phase like NASICON-type material with space group R3c. X-ray photoelectron spectroscopy and Raman spectrum confirmed the absence of impurities in samples, establishing elemental consistency. Microstructure analysis was performed using field emission scanning electron microscopy; samples displayed a granular surface with agglomeration of these grains in a radius of a few micrometers. Electrochemical impedance spectroscopy study showed that the conductivity of samples increased with increasing working temperature, and the highest conductivity values for Li1.5Al0.5Ti1.5(PO4)3 and Na1.5Al 0.5Ti1.5(PO4)3 at 150°C were found to be 3.5 × 10−4 and 5.3 × 10−4 Scm−1, respectively. Findings reinforce the suitability of these electrolytes, offering a basis for future work in solid batteries in general and for lithium-ion and sodium-ion batteries in particular.

AB - The suitability of NASICON-based M1+xAlxTi2−x(PO4)3, where M = Li, Na, and x = 0.5 solid-state electrolytes was investigated. Electrolytes were synthesized using high-temperature annealing of NH4H2PO4, TiO2, and Al2O3 compounds followed by ball milling. Synthesized samples displayed a single crystalline phase like NASICON-type material with space group R3c. X-ray photoelectron spectroscopy and Raman spectrum confirmed the absence of impurities in samples, establishing elemental consistency. Microstructure analysis was performed using field emission scanning electron microscopy; samples displayed a granular surface with agglomeration of these grains in a radius of a few micrometers. Electrochemical impedance spectroscopy study showed that the conductivity of samples increased with increasing working temperature, and the highest conductivity values for Li1.5Al0.5Ti1.5(PO4)3 and Na1.5Al 0.5Ti1.5(PO4)3 at 150°C were found to be 3.5 × 10−4 and 5.3 × 10−4 Scm−1, respectively. Findings reinforce the suitability of these electrolytes, offering a basis for future work in solid batteries in general and for lithium-ion and sodium-ion batteries in particular.

KW - activation energy

KW - diffusion mechanism

KW - electrical conductivities

KW - energy storage

KW - lithium-ion batteries

KW - polyethylene glycol

KW - sodium-ion batteries

KW - solid state electrolytes

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