The oxide known as LLZO, with nominal composition Li7La3Zr2O12, is a promising solid electrolyte for Li-based batteries due to its high Li-ion conductivity and chemical stability with respect to lithium. Solid electrolytes may also enable the use of metallic Li anodes by serving as a physical barrier that suppresses dendrite initiation and propagation during cycling. Prior linear elasticity models of the Li electrode/solid electrolyte interface suggest that the stability of this interface is highly dependent on the elastic properties of the solid separator. For example, dendritic suppression is predicted to be enhanced as the electrolyte’s shear modulus increases. In the present study a combination of first-principles calculations, acoustic impulse excitation measurements, and nanoindentation experiments are used to determine the elastic constants and moduli for high-conductivity LLZO compositions based on Al and Ta doping. The calculated and measured isotropic shear moduli are in good agreement and fall within the range of 56–61 GPa. These values are an order of magnitude larger than that for Li metal and far exceed the minimum value (∼8.5 GPa) believed to be necessary to suppress dendrite initiation. These data suggest that LLZO exhibits sufficient stiffness to warrant additional development as a solid electrolyte for Li batteries.

The indentation size effect is one of several size effects on strength for which “smaller is stronger.” Through use of geometrically self-similar indenters such as cones and pyramids, the size effect is manifested as an increase in hardness with decreasing depth of penetration and becomes important at depths of less than approximately 1 μm. For spherical indenters, the diameter of the sphere is the most important length scale; spheres with diameters of less than approximately 100 μm produce measurably higher hardnesses. We critically review experimental observations of the size effect, focusing on the behavior of crystalline metals, and examine prevailing ideas on the mechanisms responsible for the effect in light of recent experimental observations and computer simulations.

Using a high-damping thermoplastic as a standard reference material, the purpose of this work is to compare measured values of the complex modulus as determined by dynamic nanoindentation and dynamic mechanical analysis (DMA). Experiments were performed at approximately 22 • C and seven frequencies over the range 1-50 Hz. The indentation measurements were performed using a 103 µm diameter flat punch and a newly developed test method that optimizes the accuracy and precision of the measured stiffness and damping. As determined by dynamic nanoindentation, values of the storage modulus and loss factor (tangent delta) ranged from 4.2 to 10.2 MPa, and 0.28 to 1.05, respectively. Over the range 1-25 Hz, DMA confirmed the nanoindentation results to within 15% or better. Collectively, these data and the testing methods used to generate them should help future investigators make more accurate and precise measurements of the dynamic properties of viscoelastic solids using nanoindentation.

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In this paper, we describe recent advances and developments for the measurement of fracture toughness at small scales by the use of nanoindentation-based methods including techniques based on micro-cantilever, beam bending and micro-pillar splitting. A critical comparison of the techniques is made by testing a selected group of bulk and thin film materials. For pillar splitting, cohesive zone finite element simulations are used to validate a simple relationship between the critical load at failure, the pillar radius, and the fracture toughness for a range of material properties and coating/substrate combinations. The minimum pillar diameter required for nucleation and growth of a crack during indentation is also estimated. An analysis of pillar splitting for a film on a dissimilar substrate material shows that the critical load for splitting is relatively insensitive to the substrate compliance for a large range of material properties. Experimental results from a selected group of materials show good agreement between single cantilever and pillar splitting methods, while a discrepancy of ∼25% is found between the pillar splitting technique and double-cantilever testing. It is concluded that both the micro-cantilever and pillar splitting techniques are valuable methods for micro-scale assessment of fracture toughness of brittle ceramics, provided the underlying assumptions can be validated. Although the pillar splitting method has some advantages because of the simplicity of sample preparation and testing, it is not applicable to most metals because their higher toughness prevents splitting, and in this case, micro-cantilever bend testing is preferred

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The fracture toughness of thin ceramic films is an important material property that plays a role in determining the in-service mechanical performance and adhesion of this important class of engineering materials. Unfortunately, measurement of thin film fracture toughness is affected by influences from the substrate and the large residual stresses that can exist in the films. In this paper, we explore a promising new technique that potentially overcomes these issues based on nanoindentation testing of micro-pillars produced by focused ion beam milling of the films. By making the pillar diameter approximately equal to its length, the residual stress in the upper portion of the pillar is almost fully relaxed, and when indented with a sharp Berkovich indenter, the pillars fracture by splitting at reproducible loads that are readily quantified by a sudden displacement excursion in the load displacement behaviour. Cohesive finite element simulations are used for analysis and development of a simple relationship between the critical load at failure, pillar radius and fracture toughness for a given material. The main novel aspect of this work is that neither crack geometries nor crack sizes need to be measured post test. In addition, the residual stress can be measured at the same time with toughness, by comparison of the indentation results obtained on the stress-free pillars and the as-deposited film. The method is tested on three different hard coatings created by physical vapour deposition, namely titanium nitride, chromium nitride and a CrAIN/Si3N4 nanocomposite. Results compare well to independently measured values of fracture toughness for the three brittle films. The technique offers several benefits over existing methods

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