An explanation of the microcrack formation in Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 ceramics

Waetzig, Katja; Rost, Axel; Langklotz, U.; Matthey, Björn; Schilm, Jochen

doi:10.1016/j.jeurceramsoc.2016.02.042

Cited by 90 publications

(68 citation statements)

References 20 publications

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“…Therefore, LATP is obtained as a pellet with very high purity. In the literature, AlPO 4 is very commonly observed, even as traces, in the XRD patterns [24,26,27]. Its action as a resistive layer is well-known and deleterious to ionic conductivity [28].…”

Section: Resultsmentioning

confidence: 99%

Microwave-assisted reactive sintering and lithium ion conductivity of Li1.3Al0.3Ti1.7(PO4)3 solid electrolyte

Hallopeau

Brégiroux

Rousse

et al. 2018

Journal of Power Sources

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Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 (LATP) materials are made of a threedimensional framework of TiO 6 octahedra and PO 4 tetrahedra, which provides several positions for Li + ions. The resulting high ionic conductivity is promising to yield electrolytes for all-solid-state Li-ion batteries. In order to elaborate dense ceramics, conventional sintering methods often use high temperature ( 1000°C) with long dwelling times (several hours) to achieve high relative density ( 90%).In this work, an innovative synthesis and processing approach is proposed. A fast and easy processing technique called microwave-assisted reactive sintering is used to both synthesize and sinter LATP ceramics with suitable properties in one single step. Pure and crystalline LATP ceramics can be achieved in only 10 min at 890 °C starting from amorphous, compacted LATP's precursors powders. Despite a relative density of 88%, the ionic conductivity measured at ambient temperature (3.15 x 10 -4 S.cm -1 ) is among the best reported so far. The study of the activation energy for Li + conduction confirms the high quality of the ceramic (purity and crystallinity) achieved by using this new approach, thus emphasizing its interest for making ion-conducting ceramics in a simple and fast way.

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Section: Resultsmentioning

confidence: 99%

Microwave-assisted reactive sintering and lithium ion conductivity of Li1.3Al0.3Ti1.7(PO4)3 solid electrolyte

Hallopeau

Brégiroux

Rousse

et al. 2018

Journal of Power Sources

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“…To reducel ithium loss during the heat-treatmentp rocess for LATP and LAGP solid electrolyte synthesis, rapid sintering techniques have been developed:S PS, [60][61][62] FAST, [63] and MW-assisted sintering (Figure1c-e). [64,65] In principle, the SPS technique utilizes electrical currents to aid densification in ad ie with resistive heating at highr ates (> 100 8Cmin À1 ).…”

Section: Fast Sintering Techniquesmentioning

confidence: 99%

“…[87] The amount of AlPO 4 phase varies, depending upon the synthetic approaches and process parameters. At high temperatures (> 950 8C), the rhombohedral lattice structure in LATP shrinks due to the vaporization of Li 2 O, which results in the formation of AlPO 4 and TiO 2 phases [61] (Figure 4). [88] If the temperature is highert han 900 8C, the secondary phase of AlPO 4 appears, whichs uggests the loss of Al from the NaSICON-type structure.…”

Section: Secondary Phasesmentioning

confidence: 99%

“…Thus, the optimal heattreatment temperatures for solid-state synthesis are considered to be between 650 and 800 8C. [61] Figure 4. For example, if different Al sources were used as precursors in sol-gels ynthesis, [72] the LATP from Al(NO 3 ) 3 contained as mall amount of AlPO 4 ,w hereas the LATP from Al(C 3 H 7 O) 3 resulted in higherp urity.F or solution-based synthesis,K ey et al [51] clearly observed that the removal of Al from the primary phase was dependento ns intering temperatures,a sc onfirmed by means of NMR spectroscopy results.…”

Section: Secondary Phasesmentioning

confidence: 99%

“…In additiont oA lPO 4 ,L i 4 P 2 O 7 hasa lso been reported as as econdary phase in LATP powder synthesized from the Pechini method (modified sol-gel) if the calcination temperature was highert han 850 8C. [61] Reproducedw ith permission from Refs. In solid-state synthesis, increasing the sintering temperature or time leads to an increaseo ft he Al content in the LAGP structure accompanied by ad ecrease in the amount of AlPO 4 .…”

Section: Secondary Phasesmentioning

confidence: 99%

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Synthesis and Properties of NaSICON‐type LATP and LAGP Solid Electrolytes

2019

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Inorganic solid electrolytes, in comparison with their liquid counterparts, have more potential in varioust ypes of batteries due to their dual roles of ion transportation and separation. For all-solid-state batteries, solide lectrolytes bring several advantages, [1][2][3][4][5][6] such as enhanced safety,i ncreased energy density,s olid device integration, and packaging;t hese expand the operation temperature range and potentially improve cycling stabilitya nd lifetime. Moreover,i norganic solid electrolytes are also beneficial for lithium-ion batteries and lithium-air batteries, in which they functiona se ither surface modification layers or lithium-ion conductors. [7,8] In principle, ideal solid electrolytes are expected to have several features: [9][10][11][12][13][14] 1) fast ion dynamics and negligible electronic conductivity (minimum ionic conductivity of 10 À4 Scm À1 at room temperature for practical consideration);2 )a wide electrochemical potential window for battery cycling;3 )ane xceptional mechanical strength to suppress lithium dendrite growth;4 )excellent thermal stability during the cycling processes;and 5) asimple and low cost synthetic process for large-scale applications.Generally,i norganic lithium superionic conductors are divided into three categories:o xides, sulfides, and phosphates. Suc-cessfule xamples in oxidesi nclude garnet oxides, [15,16] perovskite-type oxides, [17,18] and antiperovskite oxides. [19][20][21] Sulfide solid electrolytes include Li 2 SÀP 2 S 5 , [22,23] Li 3 PS 4 , [24][25][26] Li 7 P 3 S 11 , [27,28] Li 7 PS 6 ,a nd Li 6 PS 5 X( X = Cl, Br). [29][30][31] Popular phosphate solid electrolytes include sodium superionic conductor (NaSICON)structured lithium-ion conductors, [32][33][34][35][36] such as LiTi 2 (PO 4 ) 3 (LTP), Li 1 + x Al x Ti 2Àx (PO 4 ) 3 (LATP), and Li 1 + x Al x Ge 2Àx (PO 4 ) 3 (LAGP). Many exciting discoveries of these materials have been summarized in important review papers. [2,6,[37][38][39][40] NaSICON-type solid electrolytes, such as LATP and LAGP, have marked advantages compared with sulfides and oxides: they display chemicals tabilityi na ir and/or water,a re low cost and low toxicity,a nd have great electrochemical stability with the added benefito fe asy preparation. [2,36,38] They also exhibit attractive ionic conductivities of 10 À4 -10 À3 Scm À1 at room temperature. Such features have recently caused renewed interest in these NaSICON-structured materials and much effort has been devoted to the investigation of this type of solid electrolyte, especiallyL ATPa nd LAGP.T his manuscript reviewsr ecent progress in LATP and LAGP solid electrolytes, with as pecific focus on synthetic approaches and their effects on the crystal structures, conductive properties, and applications. Herein, general synthetic methods for LATP and LAGP solid electrolytes are first introduced, followed by ac omparison of the crystal structures, phase purities, and ionic conductivities that result from different approaches. Later,t he applications of LATP and LAGP in ful...

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Role of Interfacial Defects on Electro–Chemo–Mechanical Failure of Solid‐State Electrolyte

Liu

Jiao

et al. 2023

Advanced Materials

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High‐stress field generated by electroplating of lithium (Li) in pre‐existing defects is the main reason for mechanical failure of solid‐state electrolyte because it drives crack propagation in electrolyte, followed by Li filament growth inside and even internal short‐circuit if the filament reaches another electrode. To understand the role of interfacial defects on mechanical failure of solid‐state electrolyte, an electro–chemo–mechanical model is built to visualize distribution of stress, relative damage, and crack formation during electrochemical plating of Li in defects. Geometry of interfacial defect is found as dominating factor for concentration of local stress field while semi‐sphere defect delivers less accumulation of damage at initial stage and the longest failure time for disintegration of electrolyte. Aspect ratio, as a key geometric parameter of defect, is investigated to reveal its impact on failure of electrolyte. Pyramidic defect with low aspect ratio of 0.2–0.5 shows branched region of damage near interface, probably causing surface pulverization of solid‐state electrolyte, whereas high aspect ratio over 3.0 will trigger accumulation of damage in bulk electrolyte. The correction between interfacial defect and electro–chemo–mechanical failure of solid‐state electrolyte is expected to provide insightful guidelines for interface design in high‐power‐density solid‐state Li metal batteries.

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An explanation of the microcrack formation in Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 ceramics

Cited by 90 publications

References 20 publications

Microwave-assisted reactive sintering and lithium ion conductivity of Li1.3Al0.3Ti1.7(PO4)3 solid electrolyte

Microwave-assisted reactive sintering and lithium ion conductivity of Li1.3Al0.3Ti1.7(PO4)3 solid electrolyte

Synthesis and Properties of NaSICON‐type LATP and LAGP Solid Electrolytes

Role of Interfacial Defects on Electro–Chemo–Mechanical Failure of Solid‐State Electrolyte

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