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Kinetic analysis of the second stage of the solid-phase synthesis of Li4Ti5O12 from a mechanically activated mixture of rutile and lithium carbonate
Solid State Ionics ( IF 3.2 ) Pub Date : 2020-10-23 , DOI: 10.1016/j.ssi.2020.115440
Alexander V. Zhukov , Svetlana V. Chizhevskaya , Aleksei O. Merkushkin , Ye Ko Ko Htun

The effect of mechanical activation of a mixture of micron-sized rutile and lithium carbonate in a Pulverisette-5 ball mill on the kinetics of the second stage of Li4Ti5O12 synthesis was investigated. The values of the energy of activation of the second stage of lithium pentatitanate synthesis from starting mixtures that were mechanically activated for 1 and 60 min were determined to be 463 ± 23 kJ·mol−1 and 393 ± 20 kJ·mol−1, respectively. It was shown that mechanical activation of the starting mixture leads to the destruction of lithium carbonate with the release of CO2 and an increase in the reactivity of TiO2, which strongly influences the synthesis of lithium pentatitanate. The results of our study demonstrate that mechanical activation promotes a reduction in the temperature of the first stage of lithium pentatitanate synthesis, that is, the formation of Li2TiO3, by approximately 230°С and a reduction in the temperature of the second stage, i.e., the the formation of Li4Ti5O12, by 50 °C. We show that single-phase Li4Ti5O12 with a particle size of ca. 200 nm can be successfully synthesized from a mechanically activated starting mixture at 750 °C with a 3 h holding time or at 800 °C with a 0.5 h holding time.



中文翻译:

由金红石和碳酸锂的机械活化混合物固相合成Li 4 Ti 5 O 12的第二阶段的动力学分析

研究了在Pulverisette-5球磨机中机械活化微米级金红石和碳酸锂的混合物对Li 4 Ti 5 O 12合成第二阶段动力学的影响。测定的五钛锂合成第二级的激活的能量从起始混合物进行1分钟和60分钟进行机械活化的,该值是463±23千焦耳·摩尔-1和393±20千焦·摩尔-1,分别。结果表明,起始混合物的机械活化导致碳酸锂的破坏和CO 2的释放以及TiO 2反应性的提高。,这会严重影响五钛酸锂的合成。我们的研究结果表明,机械活化可促进戊二酸锂合成第一阶段的温度降低,即形成Li 2 TiO 3约230°С,并且降低第二阶段的温度即在50℃下形成Li 4 Ti 5 O 12。我们表明,单相Li 4 Ti 5 O 12的粒度约为ca。在750°C下保持3 h或在800°C下保持0.5 h可以从机械活化的起始混合物成功合成200 nm。

更新日期:2020-10-30
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