Abstract

ObjectivesZirconia with 3 mol% yttria (3Y‐TZP) has been used for dental crowns and bridges due to its excellent mechanical behavior. Performing fracture toughness testing on this nanograin material, however, can be a challenge. For reliable results, fracture toughness testing requires an extremely sharp notch in the test specimen that closely approximates a very sharp crack. This study was to investigate an alternative method to produce nanometer‐sized notches, which are less than the average grain size of 3Y‐TZP, during the preparation of single‐edge V‐notched beam specimens and report the resulting fracture toughness value.MethodsWe present a method using focused ion beam (FIB) milling to fabricate nanometer‐sized notches in 3Y‐TZP. The notch tip is <100 nm wide, which is smaller than the grain size, and is consistent throughout the thickness of the specimen.ResultsThe FIB‐notched specimens show a much reduced average fracture toughness of 5.64 ± 1.14 MPa√m compared to 8.90 ± 0.23 MPa√m for the specimens without FIB‐notches. The FIB‐milling did not appear to create any monoclinic phase prior to fracture toughness testing. Fractures originated at the FIB‐notches, and the notch size can be readily identified post‐mortem using a microscope. A considerable amount of tetragonal‐to‐monoclinic phase transformation was observed throughout the fracture surfaces.SignificanceFIB milling provides an alternative method to fabricate nanometer‐sized notches that are smaller than the grain size of tetragonal zirconia polycrystal. The fracture toughness determined using FIB‐notches was ~5.64 MPa√m, smaller than the specimens with V‐notches fabricated using saw blades.

Highlights

  • The single-edge V-notched beam (SEVNB) method is a standard method for determination of the fracture toughness of advanced ceramics, and the precracking technique in the method is considered to be relatively easy to carry out compared to other standard methods, as long as a sufficiently small notch-root radius is created in the beam specimens (ISO 2008)

  • We developed a highly repeatable method to fabricate nanometersized notches in 3Y-TZP that are consistent through the width of a standard specimen using focused ion beam milling

  • The focused ion beam (FIB)-notches demonstrated consistent height across the entire width of the specimens, and the openings at the notch tips were consistently

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Summary

Introduction

Dental crowns and bridges made of zirconia have gained remarkable popularity due, in part, to their resistance to catastrophic failure (Bindl & Mörmann, 2002; Conrad, Seong, & Pesun, 2007; Denry &Kelly, 2008; Esquivel-Upshaw, Anusavice, Young, Jones, & Gibbs, 2004; Fradeani, Aquilano, & Corrado, 2002; Fradeani, D'Amelio, Redemagni, & Corrado, 2005; McLaren & White, 2000; Miyazaki, Nakamura, Matsumura, Ban, & Kobayashi, 2013; Raigrodski et al, 2006; Sorensen, Choi, Fanuscu, & Mito, 1998; von Steyern,J Biomed Mater Res. 2020;108B:3323–3330.wileyonlinelibrary.com/journal/jbmb 3323 LIAO ET AL.Carlson, & Nilner, 2005; Wolfart, Bohlsen, Wegner, & Kern, 2005). Tetragonal zirconia polycrystal stabilized with 3 mol% of yttria (3YTZP) preserves the metastable tetragonal phase at room temperature (Zhao & Vanderbilt, 2002), and provides superior strength and fracture toughness compared to other biomedical ceramic materials (Piconi & Maccauro, 1999). Fracture toughness value essentially represents a material's intrinsic resistance to crack extension in mode I fracture. Extensive efforts have been documented to improve fracture toughness measurement methods for dental ceramics (Kelly & Denry, 2008; Piconi & Maccauro, 1999); fracture toughness measurements for zirconia, and brittle materials in general, are nontrivial. Fenghui (2000) showed that fracture toughness reaches a constant value when the notch-tip radius is reduced to the grain diameter for notched alumina materials. The width of the notch tip should be sharpened to a submicron level in order to conduct a convincing fracture toughness test for submicron-grained zirconia

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