A preliminary investigation of fracture toughness of Li7La3Zr2O12 and its comparison to other solid Li-ionconductors

Wolfenstine, J.; Jo, Hyun Hee; Cho, Yong Hun; David, Isabel N.; Askeland, Per; Case, Eldon D.; Kim, Hyun‐Joong; Choe, Heeman; Sakamoto, Jeff

doi:10.1016/j.matlet.2013.01.021

Cited by 93 publications

(75 citation statements)

References 27 publications

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“…Dense LLZO type materials prepared by hot pressing techniques have been mechanically evaluated by ultrasound spectroscopy and indentation methods, 22,23 …”

Section: Solid Electrolyte Mechanical Considerationsmentioning

confidence: 99%

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Review—Practical Challenges Hindering the Development of Solid State Li Ion Batteries

Kerman

Luntz

Viswanathan

et al. 2017

J. Electrochem. Soc.

562

469

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Solid state electrolyte systems boasting Li + conductivity of >10 mS cm −1 at room temperature have opened the potential for developing a solid state battery with power and energy densities that are competitive with conventional liquid electrolyte systems. The primary focus of this review is twofold. First, differences in Li penetration resistance in solid state systems are discussed, and kinetic limitations of the solid state interface are highlighted. Second, technological challenges associated with processing such systems in relevant form factors are elucidated, and architectures needed for cell level devices in the context of product development are reviewed. Specific research vectors that provide high value to advancing solid state batteries are outlined and discussed. Solid state battery systems are of great interest because of potential benefits in gravimetric and volumetric energy density, operable temperature range, and safety in comparison to traditional liquid electrolyte based systems. However, unresolved fundamental issues remain in the quest to fully understand the behavior of all-solid batteries, especially in the area of electrochemical interfaces.1 There are also a number of significant engineering challenges that require methodical effort to enable a tangible product. Some transitions from academic laboratories to entrepreneurial efforts attempting to overcome these challenges remain unsuccessful in efforts to bring a product to the market.2,3 Vital parameters that require robust understanding from a product development standpoint are material cost, cell lifetime and shelf life, cell energy density on a volumetric and gravimetric basis, operable capabilities for given temperature conditions, and safety. The advantage of energy density remains to be realized in solid state electrolytes (SSEs) since most studies to date utilize thick SSEs or cathodes with low active loading compared to liquid counterparts. 4,5 Furthermore, the desire to use SSEs in conjunction with Li metal anodes requires understanding and managing the morphology of Li metal plating, which can impact volumetric energy density. Operation at both higher and lower temperature compared to conventional technologies is a significant potential advantage of SSE systems. However, reports of solid state cells achieving parity with traditional systems at room temperature or any other temperature do not currently exist. The safety, specifically decreased flammability, of SSE systems is another potential advantage but requires ongoing validation and study.6 Unlike current liquid electrolyte systems, 7 the manufacturability and material component costs of SSEs have not been well characterized, and thus the value of these features will need to be weighed accordingly with any added cost. Operating lifetime of SSEs capturing intrinsic materials parameters such as voltage stability, 8 as well as catastrophic failure modes such as shorting, 9 have been briefly investigated, but in the absence of high energy density electrode formulations and appli...

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“…Dense LLZO type materials prepared by hot pressing techniques have been mechanically evaluated by ultrasound spectroscopy and indentation methods, 22,23 …”

Section: Solid Electrolyte Mechanical Considerationsmentioning

confidence: 99%

“…Dense LLZO type materials prepared by hot pressing techniques have been mechanically evaluated by ultrasound spectroscopy and indentation methods, 22,23 and are found to exhibit an elastic modulus of 150 GPa and fracture toughness of 0. 86 of 40 GPa and fracture toughness of 0.37 MPa m 0.5 .…”

Section: Solid Electrolyte Mechanical Considerationsmentioning

confidence: 99%

Review—Practical Challenges Hindering the Development of Solid State Li Ion Batteries

Kerman

Luntz

Viswanathan

et al. 2017

J. Electrochem. Soc.

562

469

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“…Possessing those advantages, the garnet-type oxide Li 7 La 3 Zr 2 O 12 (LLZO) became a promising candidate and aroused intense interests in the past several years. [4][5][6][7][8][9][10] The disordered arrangement of Li + and Li vacancy in the cubic LLZO lattice enables the fast Li + transport along a 3D conducting pathway. [11][12][13] However, this cubic lattice in pure LLZO is not maintained at the temperatures lower than ~630 °C, and a tetragonal phase that is thermodynamically stable at room temperature exhibits poor ionic conductivity.…”

Section: Introductionmentioning

confidence: 99%

A study of suppressed formation of low-conductivity phases in doped Li₇La₃Zr₂O₁₂ garnets by in situ neutron diffraction

et al. 2015

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Doped Li7La3Zr2O12 garnets, oxide-based solids with good Li + conductivity and compatibility, show great potential as leading electrolyte material candidates for all-solid-state lithium ion batteries. However, the conductive bulk usually suffers from the presence of secondary phases and the transition towards a low-conductive tetragonal phase during synthesis. Dopants are designed to stabilize the high-conductive cubic phase and suppress the formation of the low-conductive phases. The in-situ neutron diffraction enables a direct observation of the doping effects by monitoring the phase evolutions during garnet synthesis. It reveals the reaction mechanism involving the temporary presence of intermediate phases. The offstoichiometry due to the liquid Li2CO3 evaporation leads to the residual of the low-conductive intermediate phase in the as-synthesized bulk. Proper doping of active element may alter the component of the intermediate phases and promote the completion of the reaction. While the dopants aid to stabilize most of the cubic phase, a small amount of tetragonal phase tends to form under a diffusion process. The in-situ observations provide the guideline of process optimization to suppress the formation of unwanted low-conductive phases.

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“…The sample was not immersed within oil during such experiments due to instrument constraints. However, the surfaces of samples removed from mineral oil baths immediately before testing retained an oil surface film and thus remained stable for [15][16][17][18][19][20][21][22][23][24][25][26][27][28][29][30] minutes as required for these experiments. Beyond such durations, visible oxidation reaction products were apparent in some surface regions.…”

Section: Phase and Electrochemical Characterizationmentioning

confidence: 99%

“…[22] Solid electrolyte garnet-type oxides such as LLTO and LLZO are much stiffer (E ~ 100 GPa), but likewise less brittle (K Ic ~ 0.9 to 1.6 MPa-m 1/2 when measured via Newton-scale indentation as reported herein). [10,23] To confirm the structure and conductivity of the sample, we ground the LPS to a powder form and conducted X-ray diffraction (XRD) and electrochemical impedance spectroscopy (EIS) measurements. Figure 3a shows the XRD pattern of the melt-quenched LPS sample (after grinding to powder), the same material after annealing for stress-relief, and the pattern reported by Minami et al [24] for "glassy" LPS powder obtained via the same melt-quench process.…”

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confidence: 99%

Compliant Yet Brittle Mechanical Behavior of Li₂S–P₂S₅ Lithium‐Ion‐Conducting Solid Electrolyte

McGrogan

Swamy

Bishop

et al. 2017

Advanced Energy Materials

232

134

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A preliminary investigation of fracture toughness of Li7La3Zr2O12 and its comparison to other solid Li-ionconductors

Cited by 93 publications

References 27 publications

Review—Practical Challenges Hindering the Development of Solid State Li Ion Batteries

Review—Practical Challenges Hindering the Development of Solid State Li Ion Batteries

A study of suppressed formation of low-conductivity phases in doped Li₇La₃Zr₂O₁₂ garnets by in situ neutron diffraction

Compliant Yet Brittle Mechanical Behavior of Li₂S–P₂S₅ Lithium‐Ion‐Conducting Solid Electrolyte

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A preliminary investigation of fracture toughness of Li7La3Zr2O12 and its comparison to other solid Li-ionconductors

Cited by 93 publications

References 27 publications

Review—Practical Challenges Hindering the Development of Solid State Li Ion Batteries

Review—Practical Challenges Hindering the Development of Solid State Li Ion Batteries

A study of suppressed formation of low-conductivity phases in doped Li7La3Zr2O12 garnets by in situ neutron diffraction

Compliant Yet Brittle Mechanical Behavior of Li2S–P2S5 Lithium‐Ion‐Conducting Solid Electrolyte

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A study of suppressed formation of low-conductivity phases in doped Li₇La₃Zr₂O₁₂ garnets by in situ neutron diffraction

Compliant Yet Brittle Mechanical Behavior of Li₂S–P₂S₅ Lithium‐Ion‐Conducting Solid Electrolyte