Abstract
Li1.5Al0.5Ti1.5(PO4)3 (LATP) powders were prepared from different NO x -free precursors using an aqueous-based solution-assisted solid-state reaction (SA-SSR). The sintering behavior, phase formation, microstructure and ionic conductivity of the powders were explored as a function of sintering temperature. The powders showed a relatively narrow temperature windows in which shrinkage occurred. Relative densities of 95% were reached upon heating between 900 and 960 °C. Depending on the morphological features of the primary particles, either homogeneous and intact microstructures with fine grains of about <2 µm in size or a broad grain size distribution, micro-cracks and grain cleavages were obtained, indicating the instability of the microstructure. Consequently, the ceramics with a homogeneous microstructure possessed a maximum total ionic conductivity of 0.67 mS cm−1, whereas other ceramics reached only 0.58 mS cm−1 and 0.21 mS cm−1.
Dedicated to Paul Heitjans on the occasion of his 75th birthday.
Funding source: German Federal Ministry of Education and Research (BMBF)
Award Identifier / Grant number: 03XP0109E
Acknowledgements
We thank Dr. D. Grüner (FZJ, IEK-2) for the SEM investigations, M. Andreas and V. Bader for technical assistance, and A. Hilgers for PSD and M.-T. Gerhards for DTA/TG and dilatometry measurements. We also thank our colleagues at the Central Institute of Engineering, Electronics and Analytics (ZEA-3) for the ICP-OES analysis.
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Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.
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Research funding: The results of this work are part of the project “BCT – Battery Cell Technology” funded by the German Federal Ministry of Education and Research (BMBF) under support code 03XP0109E. The authors take responsibility for the content of this publication.
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Conflict of interest statement: The authors declare no conflicts of interest regarding this article.
References
1. Zhao, E., Ma, F., Jin, Y., Kanamura, K. J. Alloys Comp. 2016, 680, 646–653, https://doi.org/10.1016/j.jallcom.2016.04.173.Suche in Google Scholar
2. Kunshina, G. B., Gromov, O. G., Lokshin, E. P., Kalinnikov, V. T. Russ. J. Inorg. Chem. 2014, 59, 424–430, https://doi.org/10.1134/s0036023614050118.Suche in Google Scholar
3. Xu, X., Wen, Z., Wu, J., Yang, J. Solid State Ionics 2007, 178, 29–34, https://doi.org/10.1016/j.ssi.2006.11.009.Suche in Google Scholar
4. Bucharsky, E. C., Schell, K. G., Hintennach, A., Hoffmann, M. J. Solid State Ionics 2015, 274, 77–82, https://doi.org/10.1016/j.ssi.2015.03.009.Suche in Google Scholar
5. Ma, Q., Xu, Q., Tsai, C.-L., Tietz, F., Guillon, O. J. Am. Ceram. Soc. 2016, 99, 410–414, https://doi.org/10.1111/jace.13997.Suche in Google Scholar
6. Key, B., Schroeder, D. J., Ingram, B. J., Vaughey, J. T. Chem. Mater. 2012, 24, 287–293, https://doi.org/10.1021/cm202773d.Suche in Google Scholar
7. Epp, V., Ma, Q., Tietz, F., Wilkening, M. Phys. Chem. Chem. Phys. 2015, 17, 32115–32121, https://doi.org/10.1039/c5cp05337d.Suche in Google Scholar PubMed
8. Vinod Chandran, C., Pristat, S., Witt, E., Tietz, F., Heitjans, P. J. Phys. Chem. C 2016, 120, 8436–8442, https://doi.org/10.1021/acs.jpcc.6b00318.Suche in Google Scholar
9. Ma, Q., Guin, M., Naqash, S., Tsai, C.-L., Tietz, F., Guillon, O. Chem. Mater. 2016, 28, 4821–4828, https://doi.org/10.1021/acs.chemmater.6b02059.Suche in Google Scholar
10. Naqash, S., Ma, Q., Tietz, F., Guillon, O. Solid State Ionics 2017, 302, 83–91, https://doi.org/10.1016/j.ssi.2016.11.004.Suche in Google Scholar
11. Davaasuren, B., Tietz, F. Solid State Ionics 2019, 338, 144–152, https://doi.org/10.1016/j.ssi.2019.05.016.Suche in Google Scholar
12. Kotobuki, M., Kobayashi, B., Koishi, M., Mizushima, T., Kakuta, N. Mater. Technol. 2014, 29, A93–A97, https://doi.org/10.1179/1753555714y.0000000181.Suche in Google Scholar
13. Degen, T., Sadki, M., Bron, E., König, U., Nénert, G. Powder Diffr. 2014, 29, S13–S18, https://doi.org/10.1017/s0885715614000840.Suche in Google Scholar
14. Hallopeau, L., Bregiroux, D., Rousse, G., Portehault, D., Stevens, P., Toussaint, G., Laberty-Robert, C. J. Power Sources 2018, 378, 48–52, https://doi.org/10.1016/j.jpowsour.2017.12.021.Suche in Google Scholar
15. Woodcock, D. A., Lightfoot, P. J. Mater. Chem. 1999, 9, 2907–2911, https://doi.org/10.1039/a904193a.Suche in Google Scholar
16. Huang, C. Y., Agrawal, D. K., McKinstry, H. A. J. Mater. Sci. 1995, 30, 3509–3514, https://doi.org/10.1007/bf00349902.Suche in Google Scholar
17. Prasada Rao, R., Maohua, C., Adams, S. J. Solid State Electrochem. 2012, 16, 3349–3354, https://doi.org/10.1007/s10008-012-1780-x.Suche in Google Scholar
18. Hupfer, T., Bucharsky, E. C., Schell, K. G., Senyshyn, A., Monchak, M., Hoffmann, M. J., Ehrenberg, H. Solid State Ionics 2016, 288, 235–239, https://doi.org/10.1016/j.ssi.2016.01.036.Suche in Google Scholar
19. Case, D., McSloy, A. J., Sharpe, R., Yeadel, S. R., Bartlett, T., Cookson, J., Dashjav, E., Tietz, F., Kumar, C. M. N., Goddard, P. Solid State Ionics 2020, 346, 115192, https://doi.org/10.1016/j.ssi.2019.115192.Suche in Google Scholar
20. Oota, T., Yamai, I. J. Am. Ceram. Soc. 1986, 69, 1–6, https://doi.org/10.1111/j.1151-2916.1986.tb04682.x.Suche in Google Scholar
21. Yamai, I., Ota, T. J. Am. Ceram. Soc. 1993, 76, 487–491, https://doi.org/10.1111/j.1151-2916.1993.tb03811.x.Suche in Google Scholar
22. Jackman, S. D., Cutler, R. A. J. Power Sources 2012, 218, 65–72, https://doi.org/10.1016/j.jpowsour.2012.06.081.Suche in Google Scholar
23. Sinclair, D. C. Bol. Soc. Esp. Cerám. Vidrio 1995, 34, 55–65.Suche in Google Scholar
24. Kotobuki, M., Koishi, M., Kato, Y. Ionics 2013, 19, 1945–1948, https://doi.org/10.1007/s11581-013-1000-4.Suche in Google Scholar
25. Rossbach, A., Tietz, F., Grieshammer, S. J. Power Sources 2018, 391, 1–9. and references therein, https://doi.org/10.1016/j.jpowsour.2018.04.059.Suche in Google Scholar
26. Kotobuki, M., Koishi, M. Ceram. Int. 2013, 39, 4645–4649, https://doi.org/10.1016/j.ceramint.2012.10.206.Suche in Google Scholar
27. Winter, E., Seipel, P., Zinkevich, T., Indris, S., Davaasuren, B., Tietz, F., Vogel, M., Z. Phys. Chem. 2022, 236, 689.10.1515/zpch-2022-1774Suche in Google Scholar
28. Lang, B., Ziebarth, B., Elsässer, C. Chem. Mater. 2015, 27, 5040–5048, https://doi.org/10.1021/acs.chemmater.5b01582.Suche in Google Scholar
Supplementary Material
The online version of this article offers supplementary material (https://doi.org/10.1515/zpch-2021-3090).
© 2021 Walter de Gruyter GmbH, Berlin/Boston
Artikel in diesem Heft
- Frontmatter
- Preface
- Special issue on the occasion of the 75th birthday of Paul Heitjans
- Contribution to Special Issue dedicated to Paul Heitjans
- Unusual cation coordination in nanostructured mullites
- A novel high entropy spinel-type aluminate MAl2O4 (M = Zn, Mg, Cu, Co) and its lithiated oxyfluoride and oxychloride derivatives prepared by one-step mechanosynthesis
- Two new quaternary copper bismuth sulfide halides: CuBi2S3Cl and CuBi2S3Br as candidates for copper ion conductivity
- Sintering behavior and ionic conductivity of Li1.5Al0.5Ti1.5(PO4)3 synthesized with different precursors
- Status and progress of ion-implanted βNMR at TRIUMF
- How Li diffusion in spinel Li[Ni1/2Mn3/2]O4 is seen with μ ±SR
- Nuclear magnetic resonance (NMR) studies of sintering effects on the lithium ion dynamics in Li1.5Al0.5Ti1.5(PO4)3
- Anion reorientations and cation diffusion in a carbon-substituted sodium nido-borate Na-7,9-C2B9H12: 1H and 23Na NMR studies
- Site preferences and ion dynamics in lithium chalcohalide solid solutions with argyrodite structure: I. A multinuclear solid state NMR study of the system Li6PS5-xSexI and of Li6AsS5I
- Site preferences and ion dynamics in lithium chalcohalide solid solutions with argyrodite structure: II. Multinuclear solid state NMR of the systems Li6PS5−x Se x Cl and Li6PS5−x Se x Br
- Independent component analysis combined with Laplace inversion of spectrally resolved spin-alignment echo/T 1 3D 7Li NMR of superionic Li10GeP2S12
- How the cation size impacts on the relaxational and diffusional dynamics of supercooled butylammonium-based ionic liquids: DPEBA–TFSI versus BTMA–TFSI
- Solid-state NMR studies of non-ionic surfactants confined in mesoporous silica
- Inorganic-organic hybrid materials based on the intercalation of radical cations: 2-(4-N-methylpyridinium)-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazol-1-oxyl-3-N-oxide in fluoromica clay
- Lithium tracer diffusion in near stoichiometric LiNi0.5Mn1.5O4 cathode material for lithium-ion batteries
- On the CaF2-BaF2 interface
- The ionic conductivity of alkali aluminum germanium phosphate glasses – comparison of Plasma CAIT with two electrode DC measurements
- Thin-film chemical expansion of ceria based solid solutions: laser vibrometry study
- Predicting conductivities of alkali borophosphate glasses based on site energy distributions derived from network former unit concentrations
- Ionic transport in K2Ti6O13
- F anion transport in nanocrystalline SmF3 and in mechanosynthesized, vacancy-rich Sm1—x BaxF3—x
- An overview of thermotransport in fluorite-related ionic oxides
Artikel in diesem Heft
- Frontmatter
- Preface
- Special issue on the occasion of the 75th birthday of Paul Heitjans
- Contribution to Special Issue dedicated to Paul Heitjans
- Unusual cation coordination in nanostructured mullites
- A novel high entropy spinel-type aluminate MAl2O4 (M = Zn, Mg, Cu, Co) and its lithiated oxyfluoride and oxychloride derivatives prepared by one-step mechanosynthesis
- Two new quaternary copper bismuth sulfide halides: CuBi2S3Cl and CuBi2S3Br as candidates for copper ion conductivity
- Sintering behavior and ionic conductivity of Li1.5Al0.5Ti1.5(PO4)3 synthesized with different precursors
- Status and progress of ion-implanted βNMR at TRIUMF
- How Li diffusion in spinel Li[Ni1/2Mn3/2]O4 is seen with μ ±SR
- Nuclear magnetic resonance (NMR) studies of sintering effects on the lithium ion dynamics in Li1.5Al0.5Ti1.5(PO4)3
- Anion reorientations and cation diffusion in a carbon-substituted sodium nido-borate Na-7,9-C2B9H12: 1H and 23Na NMR studies
- Site preferences and ion dynamics in lithium chalcohalide solid solutions with argyrodite structure: I. A multinuclear solid state NMR study of the system Li6PS5-xSexI and of Li6AsS5I
- Site preferences and ion dynamics in lithium chalcohalide solid solutions with argyrodite structure: II. Multinuclear solid state NMR of the systems Li6PS5−x Se x Cl and Li6PS5−x Se x Br
- Independent component analysis combined with Laplace inversion of spectrally resolved spin-alignment echo/T 1 3D 7Li NMR of superionic Li10GeP2S12
- How the cation size impacts on the relaxational and diffusional dynamics of supercooled butylammonium-based ionic liquids: DPEBA–TFSI versus BTMA–TFSI
- Solid-state NMR studies of non-ionic surfactants confined in mesoporous silica
- Inorganic-organic hybrid materials based on the intercalation of radical cations: 2-(4-N-methylpyridinium)-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazol-1-oxyl-3-N-oxide in fluoromica clay
- Lithium tracer diffusion in near stoichiometric LiNi0.5Mn1.5O4 cathode material for lithium-ion batteries
- On the CaF2-BaF2 interface
- The ionic conductivity of alkali aluminum germanium phosphate glasses – comparison of Plasma CAIT with two electrode DC measurements
- Thin-film chemical expansion of ceria based solid solutions: laser vibrometry study
- Predicting conductivities of alkali borophosphate glasses based on site energy distributions derived from network former unit concentrations
- Ionic transport in K2Ti6O13
- F anion transport in nanocrystalline SmF3 and in mechanosynthesized, vacancy-rich Sm1—x BaxF3—x
- An overview of thermotransport in fluorite-related ionic oxides