Mechanical characterization of a multi-layered zirconia: Flexural strength, hardness, and fracture toughness of the different layers

Abstract

This study compared the flexural strength under monotonic (static - sσ) and cyclic load application (fatigue - fσ), hardness (H) and fracture toughness (KIC) of different layers of a multi-layered zirconia (IPS e.max ZirCAD MT Multi, Ivoclar). Each layer was sectioned, classified into three groups according to yttria content (4-YSZ, 4/5-YSZ and 5-YSZ), and shaped on samples for flexural strength and fracture toughness tests (bars: 1.0 × 1.0 × 11 mm); and Vickers hardness test (plates: 1.5 × 4.0 × 5.0 mm). Flexural strength under monotonic load application (sσ; n = 10) was obtained through two different devices (three-point-bending and ball-in-hole device) and fatigue flexural strength (fσ; n = 15; initial load: 10 N; step-size: 5 N; 10,000 cycles/step) was assessed using a ball-in-hole device under cyclic load application. Vickers hardness test (n = 5), fracture toughness test (n = 10), and additional analyzes (Finite Element Analysis - FEA, Energy-dispersive X-ray spectroscopy - EDS and Scanning Electron Microscopy - SEM) were also performed. No differences were found between the different devices in the monotonic flexural strength test, and FEA showed similar tensile stress distribution for the two devices. 4-YSZ showed higher values of flexural strength under monotonic and cyclic load application modes (sσ = 1114.73 MPa; fσ = 798.84 MPa), and fracture toughness (KIC = 3.90 MPa√m). 4/5-YSZ had an intermediate sσ; however, fσ was similar to 5-YSZ (404.00–429.36 MPa) and KIC similar to 4-YSZ (KIC = 3.66 MPa√m). No statistical differences were found for hardness and Weibull modulus for fatigue flexural strength data. The amount of yttria in the layer compositions increased from 4-YSZ to 5-YSZ, and larger zirconia crystals were observed in the topographic images of 5-YSZ. Failures in the flexural strength and toughness tests started from the face subjected to tensile stress. Different layers of the multi-layered zirconia blank presented distinct mechanical properties. 4-YSZ (cervical layer) presented the highest flexural strength under monotonic and cyclic loads (fatigue), and higher fracture toughness even similar to the transition layer (4/5-YSZ). Hardness was similar between the layers. The ball-in-hole device performed similarly to the three-point bending device and can be used as an alternative to the traditional method.