Sol–Gel Route to Nanocrystalline Lithium Metasilicate Particles

Abstract

Crystalline lithium metasilicate (Li2SiO3) nanoparticles have been synthesized using a sol–gel process with tetraethylorthosilicate and lithium ethoxide as precursors. The particle size examined by using transmission electron microscopy and BET‐specific surface area techniques is in the range 5–50 nm, depending on the temperature at which the material is calcined. The crystalline Li2SiO3 forms at ambient temperature (∼40°C), and it remains in this phase after calcination at temperatures up to 850°C. The BET‐specific surface area is ∼110 m2/g for material calcined at temperatures below 500°C, decreasing to ∼29 and ∼0.7 m2/g following calcination at 700° and 850°C, respectively. Solid‐state 29Si NMR spectroscopy shows the presence of only Q2 structural units in the material. The lithium metasilicate is further characterized using differential scanning calorimetry and thermogravimetric analysis, and Fourier transform infrared spectroscopy.

Synthesis of advanced ceramics by hydrothermal crystallization and modified related methods

“…The microstructure and textural properties obtained through the surfactant-assisted hydrothermal synthesis route, suggests advantages with respect to the solid state reaction method. These pure and nano-crystalline Li 2 SiO 3 may be suitable to be used for certain applications such as CO 2 absorption [103][104][105]. Today, synthesis of lead-free piezoceramics is of strong interest when looking at a more environmentally friendly option for the fabrication of optical and acoustic devices such as optical wave-guiding and frequency doubling [116][117][118][119][120].…”

“…In general, Li 2 SiO 3 has been synthesized by the conventional solid-state reaction method, and only some chemical routes have been studied such as the sol-gel, microemulsion and combustion methods [103][104][105]. Similar to the case of other alkaline ceramics, it is complicated to prepare lithium ceramics with small particle sizes because of its tendency to sinter or to lose lithium through a sublimation process at high temperatures.…”

Surfactant-assisted hydrothermal crystallization of nanostructured lithium metasilicate (Li2SiO3) hollow spheres: (I) Synthesis, structural and microstructural characterization

“…Additionally, Li 2 SiO 3 has been reported as a promising tritium breeder material in fusion reactors [14,15], as an ionic conductor thin film [16,17] and, more recently, as a candidate for luminescent devices [18,19]. Li 2 SiO 3 has been commonly synthesized by solid-state reaction, but other chemical routes have been explored, including sol-gel, microemulsion and modified combustion techniques [20][21][22]. However, as in other ceramic systems , it is difficult to obtain ultrafine particles of lithium-based materials by conventional methods because the firing of precursor mixtures at elevated temperatures promotes sintering.…”

Synthesis of Lithium Metasilicate Powders at Low Temperature via Mechanical Milling

“…It is also a potential fast‐ion conductor material since [SiO 4 ] tetrahedral structure is found in lithium metasilicate . Furthermore, it can be used for CO 2 captures due to its fine sorption effect for CO 2 …”

“…Recently, Zhang et al . synthesized pure Li 2 SiO 3 powder with high thermal stability at a very low temperature of 40°C via sol‐gel route by using C 2 H 5 ·OLi and tetraethyl orthosilicate (TEOS) as raw materials.…”