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Open AccessArticle

A Comparison of Microscale Techniques for Determining Fracture Toughness of LiMn2O4 Particles

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Engineering Department, University of Rome “ROMA TRE”, Via della Vasca Navale 79, 00146 Rome, Italy
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Institute for Materials Science and Center for Nanointegration Duisburg-Essen (CENIDE), University of Duisburg-Essen, Universitätsstr. 15, 45141 Essen, Germany
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Robert Bosch GmbH, Robert-Bosch-Platz 1, 70839 Gerlingen-Schillerhoehe, Germany
*
Author to whom correspondence should be addressed.
Academic Editor: Matt Pharr
Materials 2017, 10(4), 403; https://doi.org/10.3390/ma10040403
Received: 14 March 2017 / Revised: 4 April 2017 / Accepted: 7 April 2017 / Published: 12 April 2017
(This article belongs to the Special Issue Advanced Nanoindentation in Materials)
Accurate estimation of fracture behavior of commercial LiMn2O4 particles is of great importance to predict the performance and lifetime of a battery. The present study compares two different microscale techniques to quantify the fracture toughness of LiMn2O4 particles embedded in an epoxy matrix. The first technique uses focused ion beam (FIB) milled micro pillars that are subsequently tested using the nanoindentation technique. The pillar geometry, critical load at pillar failure, and cohesive FEM simulations are then used to compute the fracture toughness. The second technique relies on the use of atomic force microscopy (AFM) to measure the crack opening displacement (COD) and subsequent application of Irwin’s near field theory to measure the mode-I crack tip toughness of the material. Results show pillar splitting method provides a fracture toughness value of ~0.24 MPa.m1/2, while COD measurements give a crack tip toughness of ~0.81 MPa.m1/2. The comparison of fracture toughness values with the estimated value on the reference LiMn2O4 wafer reveals that micro pillar technique provides measurements that are more reliable than the COD method. The difference is associated with ease of experimental setup, calculation simplicity, and little or no influence of external factors as associated with the COD measurements. View Full-Text
Keywords: fracture toughness; atomic force microscopy; pillar splitting; lithium-ion batteries; nanoindentation; focused ion beam fracture toughness; atomic force microscopy; pillar splitting; lithium-ion batteries; nanoindentation; focused ion beam
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MDPI and ACS Style

Mughal, M.Z.; Amanieu, H.-Y.; Moscatelli, R.; Sebastiani, M. A Comparison of Microscale Techniques for Determining Fracture Toughness of LiMn2O4 Particles. Materials 2017, 10, 403.

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