High temperature X-ray diffraction study of the formation of Na_(2)Ti_(3)O_(7) from a mixture of sodium carbonate and titanium oxide

Na2Ti3O7 has attracted much attention in the field of anode materials for Na-ion batteries thanks to its non-toxicity and very low working potential of 0.3 V vs Na0/Na+.Building a clearer picture of its formation from cheap Na_(2)CO_(3) and TiO_(2) starting materials is therefore of obvious interest.Here,we report new insights from an in-situ high temperature X-ray diffraction study conducted from room temperature to 800°C,complemented by ex-situ characterizations.We were thereby able to position the previously reported Na_(4)Ti_(5)O_(12) and Na_(2)Ti_(6)O_(13) intermediate phases in a reaction scheme involving three successive steps and temperature ranges.Shifts and/or broadening of a subset of the Na_(2)Ti_(6)O_(13) reflections suggested a combination of intra-layer disorder with the well-established ordering of successive layers.This in-situ study was carried out on reproducible mixtures of Na_(2)CO_(3) and TiO_(2) in 1:3 molar ratio prepared by spraydrying of mixed aqueous suspensions.Single-phase Na_(2)Ti_(3)O_(7) was obtained after only 8 h at 800°C in air,instead of a minimum of 20 h for a conventional solid-state route using the same precursors.Microstructure analysis revealed~15 mm diameter granules made up from rectangular rods of a fewmm length presenting electrochemical properties in line with expectations.In the absence of grinding or formation of intimate composites with conductive carbon,the specific capacity of 137 m Ah/g at C/5 decreased at higher rates.

Elaboration of a Road Material Based on Clayey Soil and Crushed Sand

To contribute to the enhancement of unconventional local materials used for road construction,this study characterizes a crushed sand 0/5,a clayey soil and the litho-stabilized material without and with hydraulic binder and determines their use in accordance with some reference specifications(CEBTP 1984).It is shown that the different components are not usable alone in pavement base.Indeed,the plasticity index obtained for the clayey soil is 21%,a value higher than the imposed standards.In addition,the grading of the 0/5 crushed sand does not fit into the range proposed by CEBTP.A combination of these two(02)components is therefore considered to obtain a suitable material usable for the sub-base.This new material does not enter any class of the CEBTP lateritic soils.In order to be used in base layer,a treatment with hydraulic binder is carried out with the intention to improve its mechanical performances.The optimal dosage of hydraulic binder to achieve the desired mechanical performance is obtained by studying the evolution of the mechanical characteristics of the mixture.After this treatment,the Bearing Ratio index of the mix increases from 37 to 223 for the optimal dosage and the dry compaction density decreases from 2.11 to 2.06 g/cm3 while the optimal water content increases from 9%to 10.1%.