Aqueous tape casting of titanium-doped lithium metazirconate (Ti-Li2ZrO3) sheets for solid-state electrolyte applications

IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS

Open Ceramics Pub Date : 2025-01-09 DOI:10.1016/j.oceram.2025.100737

Nicolás Gabriel Orsetti , Domingo Pérez-Coll , Gabriel Lorenzo , Rodrigo Moreno , Gustavo Suárez

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Abstract

Ti-doped lithium zirconate (LZTO) sheets were successfully made by aqueous tape casting, by starting from an innovative colloidal synthesis route and optimizing the colloidal processing parameters. Zeta potential and particles size measurements, together with rheological characterization, were performed to adjust the slip composition. Then, the suspension with 1.0 wt% of ammonium polyacrylate dispersant (APA) and solid loading of 31 vol.% resulted in flat and flexible sheets, thinner than 450 µm, by adding 20 wt% of acrylic binder emulsion. After annealing at 1150 °C/15 h, LZTO sheets densified up to 85.5 %, presented a microstructure with grains of 6.4 µm in diameter, and exhibited electrical conductivity values in the order of 10⁻⁷, 10⁻⁶ and 10⁻⁵ S·cm⁻¹ at 350, 450 and 600 °C, respectively. Besides, XRD phase analysis revealed monoclinic Li₂ZrO₃ and minor ZrO₂ impurities originated from Li₂O volatilization during sintering, but no sign of TiO₂ segregation, indicating the formation of Li₂Zr_1-XTi_XO₃ solid solution.

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用于固态电解质应用的掺钛偏锆酸锂（Ti-Li2ZrO3）片材的水带铸造

从创新的胶体合成路线出发，优化胶体工艺参数，成功制备了掺杂钛的锆酸锂（LZTO）片材。Zeta电位和颗粒大小的测量，连同流变特性，进行调整滑移组成。然后，加入20%的丙烯酸粘合剂乳液，以1.0 wt%的聚丙烯酸铵分散剂（APA）和31 vol.%的固体负载为悬浮液，得到厚度小于450µm的扁平柔性片材。在1150°C/15 h退火后，LZTO片致密度高达85.5%，晶粒直径为6.4µm，在350°C、450°C和600°C时的电导率分别为10−7、10−6和10−5 S·cm−1。此外，XRD物相分析显示Li2ZrO3为单斜晶型，少量的ZrO2杂质来源于烧结过程中Li2O的挥发，但没有TiO2偏析的迹象，说明形成了Li2Zr1-XTiXO3固溶体。

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