Elaboration of controlled size Li1.5Al0.5Ge1.5(PO4)3 crystallites from glass-ceramics

Kubanska, Agnieszka; Castro, Laurent; Tortet, L.; Schäf, O.; Dollé, Mickaël; Bouchet, Renaud

doi:10.1016/j.ssi.2014.07.013

Cited by 44 publications

(25 citation statements)

References 23 publications

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“…The evolution of pellet thickness during the heat treatment is also illustrated in Figure 3 (note that here positive displacement corresponds to reduction in thickness). The measured volume change coincides with LAGP crystallization peak reported previously by differential scanning calorimetry (Kubanska et al, 2014;Yang et al, 2015). The crystallization process resulted in highly porous bodies of agglomerated crystalline powder that were subsequently reground by hand in a mortar.…”

Section: Materials Synthesis and Crystallizationsupporting

confidence: 87%

“…Resistively heating the sample itself, a process limited to electronically conductive materials is even more effective than traditional SPS but requires an SPS furnace with additional complexity of the die structure . SPS sintering of LAGP has been reported, but the achieved density was only 87% of theoretical, and the 20°C conductivity was measured to be 3.3 × 10 −5 S cm −1 (Kubanska et al, 2014), a much lower value than what is commonly reported for such a density (Mariappan et al, 2011). It is notable that an additional, though low intensity, peak appears in the X-ray diffraction (XRD) pattern of the sample after SPS, corresponding to the most intense peak of AlPO4, an insulating secondary phase, though a causal connection was not asserted.…”

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confidence: 95%

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Improving NASICON Sinterability through Crystallization under High-Frequency Electrical Fields

Lisenker

Stoldt

2016

Front. Energy Res.

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The effect of high-frequency (HF) electric fields on the crystallization and sintering rates of a lithium aluminum germanium phosphate (LAGP) ion conducting ceramic was investigated. LAGP with the nominal composition Li1.5Al0.5Ge1.5(PO4)3 was crystallized and sintered, both conventionally and under effect of electrical field. Electrical field application, of 300 V/cm at 1 MHz, produced up to a 40% improvement in sintering rate of LAGP that was crystallized and sintered under the HF field. Heat sink effect of the electrodes appears to arrest thermal runaway and subsequent flash behavior. Sintered pellets were characterized using X-ray diffraction, scanning electron microscope, TEM, and electrochemical impedance spectroscopy to compare conventionally and field-sintered processes. The as-sintered structure appears largely unaffected by the field as the sintering curves tend to converge beyond initial stages of sintering. Differences in densities and microstructure after 1 h of sintering were minor with measured sintering strains of 31 vs. 26% with and without field, respectively. Ionic conductivity of the sintered pellets was evaluated, and no deterioration due to the use of HF field was noted, though capacitance of grain boundaries due to secondary phases was significantly increased.

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Section: Materials Synthesis and Crystallizationsupporting

confidence: 87%

mentioning

confidence: 95%

Improving NASICON Sinterability through Crystallization under High-Frequency Electrical Fields

Lisenker

Stoldt

2016

Front. Energy Res.

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“…On the other hand, it was not possible to perform the ECM analysis at the higher temperatures on the impedance plots since the semicircles representing the grains and grain boundary curves were stopped at 40 °C and no longer shown. Higher than this temperature, the grains contribution will shift to higher frequencies and it will be hardly observed and separated from the grain boundaries contribution in the used available measured frequencies range [15]. …”

Section: Resultsmentioning

confidence: 99%

“…The total resistance of the sample is consisting of the grains and grain boundaries resistances. The high frequency semi-circle can be attributed to the LAGP grains conductivity while the low frequency to the grain boundaries contribution [15,57]. From Table 4, it is clear that both the grains and the grain-boundary ionic conductivities values of the MW optimized sample are significantly higher than their corresponding values of the conventionally optimized sample.…”

Section: Resultsmentioning

confidence: 99%

“…A further unique and important issue for the transport processes in ceramic electrolytes is the effect of the microstructure [13,14] since grain boundaries as well as arrangement and size of the grains can be adjusted by a proper heat treatment, which will affect the overall ionic properties. LAGP solid electrolytes have been prepared via many different routes such as melt-quenching method [11,15,16], conventional powder sintering [17,18] and sol-gel methods [19,20]. LAGP synthesized from different routes had showed ionic conductivities values in the range of 10 −4 –10 −5 S·cm −1 at room temperature.…”

Section: Introductionmentioning

confidence: 99%

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Microwave Crystallization of Lithium Aluminum Germanium Phosphate Solid-State Electrolyte

et al. 2016

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Lithium aluminum germanium phosphate (LAGP) glass-ceramics are considered as promising solid-state electrolytes for Li-ion batteries. LAGP glass was prepared via the regular conventional melt-quenching method. Thermal, chemical analyses and X-ray diffraction (XRD) were performed to characterize the prepared glass. The crystallization of the prepared LAGP glass was done using conventional heating and high frequency microwave (MW) processing. Thirty GHz microwave (MW) processing setup were used to convert the prepared LAGP glass into glass-ceramics and compared with the conventionally crystallized LAGP glass-ceramics that were heat-treated in an electric conventional furnace. The ionic conductivities of the LAGP samples obtained from the two different routes were measured using impedance spectroscopy. These samples were also characterized using XRD and scanning electron microscopy (SEM). Microwave processing was successfully used to crystallize LAGP glass into glass-ceramic without the aid of susceptors. The MW treated sample showed higher total, grains and grain boundary ionic conductivities values, lower activation energy and relatively larger-grained microstructure with less porosity compared to the corresponding conventionally treated sample at the same optimized heat-treatment conditions. The enhanced total, grains and grain boundary ionic conductivities values along with the reduced activation energy that were observed in the MW treated sample was considered as an experimental evidence for the existence of the microwave effect in LAGP crystallization process. MW processing is a promising candidate technology for the production of solid-state electrolytes for Li-ion battery.

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Progress and Perspectives of Lithium Aluminum Germanium Phosphate‐Based Solid Electrolytes for Lithium Batteries

Zhang

Liu

Xie

et al. 2023

Adv Funct Materials

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Solid‐state lithium batteries are considered promising energy storage devices due to their superior safety and higher energy density than conventional liquid electrolyte‐based batteries. Lithium aluminum germanium phosphate (LAGP), with excellent stability in air and good ionic conductivity, has gained tremendous attention over the past decades. However, the poor interface compatibility with Li anode, slow Li‐ion conduction in thick pellets, and high‐temperature sintering procedure limit the further development of LAGP solid electrolytes in practical applications. This review comprehensively summarizes the crystal structure, Li‐ion conducting mechanism, and various synthesis methods, especially the latest thin‐film preparation approach. The underlying reason for Li/LAGP interfacial instability is identified, followed by several advanced interface engineering strategies, for example, introducing a functional interlayer. The integration design of LAGP‐based solid electrolytes and cathode is also highlighted to enable high‐loading cathodes. Additionally, recent progress of lithium‐oxygen and lithium‐sulfur batteries with LAGP‐based solid electrolytes is discussed. Moreover, the different Li‐ion migration pathways, preparation procedures, and electrochemical performance of polymer‐LAGP composite solid electrolytes in Li‐ion batteries are introduced. Lastly, the remaining challenges and opportunities are proposed to encourage more efforts in this field. This review aims to provide fundamental insights and promising directions toward practical LAGP‐based solid‐state batteries.

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Elaboration of controlled size Li1.5Al0.5Ge1.5(PO4)3 crystallites from glass-ceramics

Cited by 44 publications

References 23 publications

Improving NASICON Sinterability through Crystallization under High-Frequency Electrical Fields

Improving NASICON Sinterability through Crystallization under High-Frequency Electrical Fields

Microwave Crystallization of Lithium Aluminum Germanium Phosphate Solid-State Electrolyte

Progress and Perspectives of Lithium Aluminum Germanium Phosphate‐Based Solid Electrolytes for Lithium Batteries

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