Biaxial strength under fatigue of 4YSZ: Surface treatment and resin cement viscosity effects

Kétlin Fagundes Teixeira; Fernanda Cocco; Pablo Machado Soares; Gabriel Kalil Rocha Pereira; Cornelis Johannes Kleverlaan; João Paulo Mendes Tribst; Luiz Felipe Valandro; Ana Carolina Cadore-Rodrigues

doi:10.1371/journal.pone.0349754

Biaxial strength under fatigue of 4YSZ: Surface treatment and resin cement viscosity effects

Kétlin Fagundes Teixeira
, Fernanda Cocco
, Pablo Machado Soares
, Gabriel Kalil Rocha Pereira
, Cornelis Johannes Kleverlaan
, João Paulo Mendes Tribst
, Luiz Felipe Valandro
, Ana Carolina Cadore-Rodrigues

Research output: Contribution to Journal › Article › Academic › peer-review

Abstract

This study aimed to investigate the effect of different surface treatments combined with high- or low-viscosity resin cements on the biaxial flexural strength of 4YSZ ceramics. Discs of 4YSZ (IPS e.max ZirCAD MT, Ivoclar AG; 15 mm diameter, 1.2 mm thickness) were prepared, subjected to CAD/CAM milling simulation using #220 silicon carbide papers, and divided into 10 groups according to two factors: "Surface Treatment" - Control (CTRL, no treatment); air abrasion with 45 µm (AB45) or 110 µm (AB110) alumina oxide particles; and glaze either followed (GLZ + HF) or not (GLZ) by 10% hydrofluoric acid; and "Resin Cement Viscosity" - High (H) or Low (L). The discs were treated, luted with resin cement, and subjected to two monotonic tests (n = 2) to determine fatigue parameters, followed by biaxial fatigue testing (n = 15; piston-on-three-balls; 20 Hz; 10,000 cycles; initial stress: 75 MPa; increments of 25 MPa). Topography, fractography, and surface roughness analyses were also performed. Surface treatment significantly influenced fatigue performance (p < 0.05, F = 60.25), whereas resin cement viscosity and its interaction with surface treatment did not show significant effects (p > 0.05, F = 0.86; p > 0.05, F = 0.07). The GLZ groups exhibited the highest flexural strength (H/L-GLZ: 382-396 MPa), followed by intermediate values in CTRL (H/L-CTRL: 285-288 MPa), AB45 (H/L-AB45: 310-315 MPa), and GLZ + HF (H/L: 273-280 MPa), while AB110 groups presented the lowest strength (H/L: 205-210 MPa). Surface roughness was lower for GLZ (Ra: 1.44 µm) and GLZ + HF (Ra: 1.38 µm) compared to AB45 (Ra: 1.83 µm) and AB110 (Ra: 1.69 µm). GLZ produced smooth and homogeneous surfaces, GLZ + HF led to areas partially exposed by acid, and AB110 caused more pronounced surface defects than AB45. Hence, the GLZ treatment offered superior fatigue performance; AB45 and GLZ + HF showed behavior similar to CTRL, whereas AB110 impaired mechanical performance. Resin cement viscosity had no significant influence on fatigue strength.

Original language	English
Article number	e0349754
Journal	PLoS ONE
Volume	21
Issue number	5
Early online date	28 May 2026
DOIs	https://doi.org/10.1371/journal.pone.0349754
Publication status	Published - May 2026

Bibliographical note

Copyright: © 2026 Teixeira et al. This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.

Funding

Funding: This work is part of the fulfillment of the requirements for the MSci degree (K.F.T.) in the Post-Graduate Program in Oral Sciences at the Faculty of Dentistry, Federal University of Santa Maria (Rio Grande do Sul State, Brazil). This research was partially financed by the Brazilian Federal Agency for Coordination of Improvement of Higher Education Personnel – CAPES (Finance Code 001 for K.F.T. Master’s scholarship); by the Research Support Foundation of the State of Rio Grande do Sul – FAPERGS (#2551-0000152-7/2023 for A.C.R. Post-doctoral scholarship); and by the Brazilian National Council for Scientific and Technological Development – CNPq (#304665/2022-3 for G.K.R.P research grant; and #308427/2021-1 for L.F.V research grant; #442272/2023-5). Furthermore, we extend our heartfelt gratitude to Ivoclar AG in providing some of the materials used in this research. It is important to emphasize that the contribution of these institutions was limited to financial support, with no involvement in the study's design, data collection or analysis, publication decisions, or manuscript preparation.

Funders	Funder number
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior
Fundação de Amparo à Pesquisa do Estado do Rio Grande do Sul	2551-0000152-7/2023
Conselho Nacional de Desenvolvimento Científico e Tecnológico	304665/2022-3, 442272/2023-5, 308427/2021-1

Keywords

Resin Cements/chemistry
Viscosity
Surface Properties
Materials Testing
Flexural Strength
Stress, Mechanical
Ceramics/chemistry
Zirconium/chemistry

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Cite this

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title = "Biaxial strength under fatigue of 4YSZ: Surface treatment and resin cement viscosity effects",

abstract = "This study aimed to investigate the effect of different surface treatments combined with high- or low-viscosity resin cements on the biaxial flexural strength of 4YSZ ceramics. Discs of 4YSZ (IPS e.max ZirCAD MT, Ivoclar AG; 15 mm diameter, 1.2 mm thickness) were prepared, subjected to CAD/CAM milling simulation using \#220 silicon carbide papers, and divided into 10 groups according to two factors: {"}Surface Treatment{"} - Control (CTRL, no treatment); air abrasion with 45 µm (AB45) or 110 µm (AB110) alumina oxide particles; and glaze either followed (GLZ + HF) or not (GLZ) by 10\% hydrofluoric acid; and {"}Resin Cement Viscosity{"} - High (H) or Low (L). The discs were treated, luted with resin cement, and subjected to two monotonic tests (n = 2) to determine fatigue parameters, followed by biaxial fatigue testing (n = 15; piston-on-three-balls; 20 Hz; 10,000 cycles; initial stress: 75 MPa; increments of 25 MPa). Topography, fractography, and surface roughness analyses were also performed. Surface treatment significantly influenced fatigue performance (p < 0.05, F = 60.25), whereas resin cement viscosity and its interaction with surface treatment did not show significant effects (p > 0.05, F = 0.86; p > 0.05, F = 0.07). The GLZ groups exhibited the highest flexural strength (H/L-GLZ: 382-396 MPa), followed by intermediate values in CTRL (H/L-CTRL: 285-288 MPa), AB45 (H/L-AB45: 310-315 MPa), and GLZ + HF (H/L: 273-280 MPa), while AB110 groups presented the lowest strength (H/L: 205-210 MPa). Surface roughness was lower for GLZ (Ra: 1.44 µm) and GLZ + HF (Ra: 1.38 µm) compared to AB45 (Ra: 1.83 µm) and AB110 (Ra: 1.69 µm). GLZ produced smooth and homogeneous surfaces, GLZ + HF led to areas partially exposed by acid, and AB110 caused more pronounced surface defects than AB45. Hence, the GLZ treatment offered superior fatigue performance; AB45 and GLZ + HF showed behavior similar to CTRL, whereas AB110 impaired mechanical performance. Resin cement viscosity had no significant influence on fatigue strength.",

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note = "Copyright: {\textcopyright} 2026 Teixeira et al. This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.",

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month = may,

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T1 - Biaxial strength under fatigue of 4YSZ

T2 - Surface treatment and resin cement viscosity effects

AU - Teixeira, Kétlin Fagundes

AU - Cocco, Fernanda

AU - Soares, Pablo Machado

AU - Pereira, Gabriel Kalil Rocha

AU - Kleverlaan, Cornelis Johannes

AU - Tribst, João Paulo Mendes

AU - Valandro, Luiz Felipe

AU - Cadore-Rodrigues, Ana Carolina

N1 - Copyright: © 2026 Teixeira et al. This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.

PY - 2026/5

Y1 - 2026/5

N2 - This study aimed to investigate the effect of different surface treatments combined with high- or low-viscosity resin cements on the biaxial flexural strength of 4YSZ ceramics. Discs of 4YSZ (IPS e.max ZirCAD MT, Ivoclar AG; 15 mm diameter, 1.2 mm thickness) were prepared, subjected to CAD/CAM milling simulation using #220 silicon carbide papers, and divided into 10 groups according to two factors: "Surface Treatment" - Control (CTRL, no treatment); air abrasion with 45 µm (AB45) or 110 µm (AB110) alumina oxide particles; and glaze either followed (GLZ + HF) or not (GLZ) by 10% hydrofluoric acid; and "Resin Cement Viscosity" - High (H) or Low (L). The discs were treated, luted with resin cement, and subjected to two monotonic tests (n = 2) to determine fatigue parameters, followed by biaxial fatigue testing (n = 15; piston-on-three-balls; 20 Hz; 10,000 cycles; initial stress: 75 MPa; increments of 25 MPa). Topography, fractography, and surface roughness analyses were also performed. Surface treatment significantly influenced fatigue performance (p < 0.05, F = 60.25), whereas resin cement viscosity and its interaction with surface treatment did not show significant effects (p > 0.05, F = 0.86; p > 0.05, F = 0.07). The GLZ groups exhibited the highest flexural strength (H/L-GLZ: 382-396 MPa), followed by intermediate values in CTRL (H/L-CTRL: 285-288 MPa), AB45 (H/L-AB45: 310-315 MPa), and GLZ + HF (H/L: 273-280 MPa), while AB110 groups presented the lowest strength (H/L: 205-210 MPa). Surface roughness was lower for GLZ (Ra: 1.44 µm) and GLZ + HF (Ra: 1.38 µm) compared to AB45 (Ra: 1.83 µm) and AB110 (Ra: 1.69 µm). GLZ produced smooth and homogeneous surfaces, GLZ + HF led to areas partially exposed by acid, and AB110 caused more pronounced surface defects than AB45. Hence, the GLZ treatment offered superior fatigue performance; AB45 and GLZ + HF showed behavior similar to CTRL, whereas AB110 impaired mechanical performance. Resin cement viscosity had no significant influence on fatigue strength.

AB - This study aimed to investigate the effect of different surface treatments combined with high- or low-viscosity resin cements on the biaxial flexural strength of 4YSZ ceramics. Discs of 4YSZ (IPS e.max ZirCAD MT, Ivoclar AG; 15 mm diameter, 1.2 mm thickness) were prepared, subjected to CAD/CAM milling simulation using #220 silicon carbide papers, and divided into 10 groups according to two factors: "Surface Treatment" - Control (CTRL, no treatment); air abrasion with 45 µm (AB45) or 110 µm (AB110) alumina oxide particles; and glaze either followed (GLZ + HF) or not (GLZ) by 10% hydrofluoric acid; and "Resin Cement Viscosity" - High (H) or Low (L). The discs were treated, luted with resin cement, and subjected to two monotonic tests (n = 2) to determine fatigue parameters, followed by biaxial fatigue testing (n = 15; piston-on-three-balls; 20 Hz; 10,000 cycles; initial stress: 75 MPa; increments of 25 MPa). Topography, fractography, and surface roughness analyses were also performed. Surface treatment significantly influenced fatigue performance (p < 0.05, F = 60.25), whereas resin cement viscosity and its interaction with surface treatment did not show significant effects (p > 0.05, F = 0.86; p > 0.05, F = 0.07). The GLZ groups exhibited the highest flexural strength (H/L-GLZ: 382-396 MPa), followed by intermediate values in CTRL (H/L-CTRL: 285-288 MPa), AB45 (H/L-AB45: 310-315 MPa), and GLZ + HF (H/L: 273-280 MPa), while AB110 groups presented the lowest strength (H/L: 205-210 MPa). Surface roughness was lower for GLZ (Ra: 1.44 µm) and GLZ + HF (Ra: 1.38 µm) compared to AB45 (Ra: 1.83 µm) and AB110 (Ra: 1.69 µm). GLZ produced smooth and homogeneous surfaces, GLZ + HF led to areas partially exposed by acid, and AB110 caused more pronounced surface defects than AB45. Hence, the GLZ treatment offered superior fatigue performance; AB45 and GLZ + HF showed behavior similar to CTRL, whereas AB110 impaired mechanical performance. Resin cement viscosity had no significant influence on fatigue strength.

KW - Resin Cements/chemistry

KW - Viscosity

KW - Surface Properties

KW - Materials Testing

KW - Flexural Strength

KW - Stress, Mechanical

KW - Ceramics/chemistry

KW - Zirconium/chemistry

U2 - 10.1371/journal.pone.0349754

DO - 10.1371/journal.pone.0349754

M3 - Article

C2 - 42207817

SN - 1932-6203

VL - 21

JO - PLoS ONE

JF - PLoS ONE

IS - 5

M1 - e0349754

ER -

Biaxial strength under fatigue of 4YSZ: Surface treatment and resin cement viscosity effects

Abstract

Bibliographical note

Funding

Keywords

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