1. Quantifying Li-content for compositional tailoring of lithium ferrite ceramics
- Author
-
Granados-Miralles, C., Serrano, A., Prieto, P., Guzmán-Mínguez, J. C., Prieto, J. E., Friedel, A. M., García-Martín, Eduardo, Fernández, J. F., Quesada, A., Ministerio de Ciencia e Innovación (España), Comunidad de Madrid, and European Science Foundation
- Subjects
Sintered ceramics ,Confocal Raman spectroscopy ,Magnetic properties ,Rietveld analysis ,Materials Chemistry ,Ceramics and Composites ,Lithium quantification - Abstract
9 pags., 6 figs., 3 tabs., Owing to their multiple applications, lithium ferrites are relevant materials for several emerging technologies. For instance, LiFeO2 has been spotted as an alternative cathode material in Li-ion batteries, while LiFe5O8 is the lowest damping ferrite, holding promise in the field of spintronics. The Li-content in lithium ferrites has been shown to greatly affect the physical properties, and in turn, the performance of functional devices based on these materials. Despite this, lithium content is rarely accurately quantified, as a result of the low number of electrons in Li hindering its identification by means of routine materials characterization methods. In the present work, magnetic lithium ferrite powders with Li:Fe ratios of 1:1, 1:3 and 1:5 have been synthesized, successfully obtaining phase-pure materials (LiFeO2 and LiFe5O8), as well as a controlled mixture of both phases. The powders have been compacted and subsequently sintered by thermal treatment (Tmax = 1100 °C) to fabricate dense pellets which preserve the original Li:Fe ratios. Li-content on both powders and pellets has been determined by two independent methods: (i) Rutherford backscattering spectroscopy combined with nuclear reaction analysis and (ii) Rietveld analysis of powder X-ray diffraction data. With good agreement between both techniques, it has been confirmed that the Li:Fe ratios employed in the synthesis are maintained in the sintered ceramics. The same conclusion is drawn from spatially-resolved confocal Raman microscopy experiments on regions of a few microns. Field emission scanning electron microscopy has evidenced the substantial grain growth taking place during the sintering process – mean particle sizes rise from ≈ 600 nm in the powders up to 3.8(6) µm for dense LiFeO2 and 10(2) µm for LiFe5O8 ceramics. Additionally, microstructural analysis has revealed trapped pores inside the grains of the sintered ceramics, suggesting that grain boundary mobility is governed by surface diffusion. Vibrating sample magnetometry on the ceramic samples has confirmed the expected soft ferrimagnetic behavior of LiFe5O8 (with Ms = 61.5(1) Am2/kg) and the paramagnetic character of LiFeO2 at room temperature. A density of 92.7(6)% is measured for the ceramics, ensuring the mechanical integrity required for both their direct utilization in bulk shape and their use as targets for thin-film deposition., This work has been supported by grants RTI2018-095303-B-C51 and RTI2018-095303-A-C52 funded by MCIN/AEI/ 10.13039/501100011033 and by “ERDF A way of making Europe” and grants PID20210124585NB-C31, PID2021–124585NB-C32 and PID2021-124585NB-C33 funded by MCIN/AEI/ 10.13039/501100011033 and by the “European Union NextGenerationEU/PRTR”. C.G.-M. acknowledges financial support from grant FJC2018–035532-I funded by MCIN/AEI/ 10.13039/501100011033 and grant RYC2021–031181-I funded by MCIN/AEI/10.13039/501100011033 and by the “European Union NextGeneration EU/PRTR”. A.S. acknowledges financial support from the Comunidad de Madrid for an “Atracción de Talento Investigador” contract No. 2017-t2/IND5395 and grant RYC2021-031236-I funded by MCIN/AEI/10.13039/501100011033 and by the “European Union NextGenerationEU/PRTR”. A.Q. acknowledges financial support from grant RYC-2017023320 funded by MCIN/AEI/ 10.13039/501100011033 and by “ESF Investing in your future”. The authors acknowledge support from CMAM for beamtime proposals with codes STD019/20, STD026/20 and STD033/20.
- Published
- 2023
- Full Text
- View/download PDF