Mechanochemical Activation and Sodium Intercalation in the NaTi2(PO4)3 NASICON Structure

Abstract

NaTi2(PO4)3 , a NASICON-type sodium titanium phosphate (NTP), is a promising candidate for sodium-ion energy storage due to its robust structural and electrochemical properties. This study explores the impact of mechanochemical activation (MCA) on NTP synthesized via high-temperature methods, with a focus on sodium intercalation behaviour under various milling conditions. Sodiation experiments were performed in suspension using different sodium sources and the resulting structural and compositional changes after activation and the mean sodium content (<x>) in Na x Ti 2 (PO 4 ) 3 were determined by powder X-ray diffraction (PXRD) combined with Rietveld refinement as well as scanning electron microscopy (SEM), physisorption isotherm measurements, inductively coupled plasma mass spectrometry (ICP-MS), Raman spectroscopy and solid-state NMR. While MCA did not induce a phase transformation, extended milling times led to reduced crystallite sizes and increased structural disorder. The extent of sodium incorporation was strongly influenced by both the milling duration and the chemical nature of the sodium source, particularly its ability to reduce titanium.The highest sodium content of 3.5 approaching the theoretical maximum of 4.0 (Na4Ti2(PO4)3) was achieved using sodium naphthalene as the sodiation reagent.

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Article information

Article type
Paper
Submitted
01 Jul 2025
Accepted
01 Oct 2025
First published
02 Oct 2025
This article is Open Access
Creative Commons BY license

RSC Mechanochem., 2025, Accepted Manuscript

Mechanochemical Activation and Sodium Intercalation in the NaTi2(PO4)3 NASICON Structure

T. B. Straub, G. Kickelbick and E. C. J. Gießelmann, RSC Mechanochem., 2025, Accepted Manuscript , DOI: 10.1039/D5MR00090D

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