{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2025,11,24]],"date-time":"2025-11-24T16:42:00Z","timestamp":1764002520517,"version":"build-2065373602"},"reference-count":46,"publisher":"MDPI AG","issue":"6","license":[{"start":{"date-parts":[[2022,3,10]],"date-time":"2022-03-10T00:00:00Z","timestamp":1646870400000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Materials"],"abstract":"<jats:p>There is still a lack of consensus concerning the recommended etching concentration, application time and type of silane when bonding lithium disilicate-reinforced glass ceramics manufactured by CAD\/CAM. The purpose of this study was thus to conduct an in vitro study which investigates the influence of hydrofluoric acid (HF) concentration, etching time and silane type on the microtensile bond strength (\u03bcTBS) of lithium disilicate to resin composites. Thirty-nine IPS e.max CAD blocks were randomly divided between thirteen groups (n = 3). The variables were HF concentration (9.5 or 4.9%), etching time (20 or 60 s) and silane type (Bis-Silane, Monobond Plus and ESPE Sil Silane). The blocks were cut into beams, aged for 10,000 cycles in a thermocycler and submitted to tensile stress to determine \u03bcTBS. A control group featuring the Monobond Etch &amp; Prime (MEP) agent that combines etching\/silanisation into a simultaneous process was also added. This group was discarded from the analysis due to only having pre-test failures. The data were analysed using a three-way ANOVA (\u03b1 = 0.05). The HF concentration, etching time and silane type significantly influenced \u03bcTBS (p &lt; 0.001). Significant interactions between time and silane type (p = 0.004), HF concentration and silane type (p &lt; 0.001) and among the three factors (p &lt; 0.001) were noted. Etching lithium disilicate with 9.5% HF (60 s), followed by the application of Bis-Silane, resulted in the highest \u03bcTBS (16.6 \u00b1 9.0 MPa). The highest concentration and etching time under study, combined with a two-part silane, resulted in the highest bond strength, while the application of MEP showed a complete pre-test failure.<\/jats:p>","DOI":"10.3390\/ma15062045","type":"journal-article","created":{"date-parts":[[2022,3,10]],"date-time":"2022-03-10T20:19:10Z","timestamp":1646943550000},"page":"2045","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":12,"title":["Increasing Acid Concentration, Time and Using a Two-Part Silane Potentiates Bond Strength of Lithium Disilicate\u2013Reinforced Glass Ceramic to Resin Composite: An Exploratory Laboratory Study"],"prefix":"10.3390","volume":"15","author":[{"given":"Matilde","family":"Almiro","sequence":"first","affiliation":[{"name":"Department of Conservative Dentistry, Instituto Universit\u00e1rio Egas Moniz (IUEM), Monte de Caparica, 2829-511 Almada, Portugal"}]},{"given":"Beatriz","family":"Marinho","sequence":"additional","affiliation":[{"name":"Department of Conservative Dentistry, Instituto Universit\u00e1rio Egas Moniz (IUEM), Monte de Caparica, 2829-511 Almada, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7902-6104","authenticated-orcid":false,"given":"Ant\u00f3nio H. S.","family":"Delgado","sequence":"additional","affiliation":[{"name":"Centro de Investiga\u00e7\u00e3o Interdisciplinar Egas Moniz (CiiEM), Instituto Universit\u00e1rio Egas Moniz (IUEM), Monte de Caparica, 2829-511 Almada, Portugal"},{"name":"Division of Biomaterials and Tissue Engineering, Eastman Dental Institute, University College London (UCL), London NW3 2PF, UK"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7659-4392","authenticated-orcid":false,"given":"Jo\u00e3o","family":"Rua","sequence":"additional","affiliation":[{"name":"Centro de Investiga\u00e7\u00e3o Interdisciplinar Egas Moniz (CiiEM), Instituto Universit\u00e1rio Egas Moniz (IUEM), Monte de Caparica, 2829-511 Almada, Portugal"}]},{"given":"Paulo","family":"Monteiro","sequence":"additional","affiliation":[{"name":"Centro de Investiga\u00e7\u00e3o Interdisciplinar Egas Moniz (CiiEM), Instituto Universit\u00e1rio Egas Moniz (IUEM), Monte de Caparica, 2829-511 Almada, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8095-0107","authenticated-orcid":false,"given":"In\u00eas Caetano","family":"Santos","sequence":"additional","affiliation":[{"name":"Centro de Investiga\u00e7\u00e3o Interdisciplinar Egas Moniz (CiiEM), Instituto Universit\u00e1rio Egas Moniz (IUEM), Monte de Caparica, 2829-511 Almada, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8482-5936","authenticated-orcid":false,"given":"Lu\u00eds","family":"Proen\u00e7a","sequence":"additional","affiliation":[{"name":"Centro de Investiga\u00e7\u00e3o Interdisciplinar Egas Moniz (CiiEM), Instituto Universit\u00e1rio Egas Moniz (IUEM), Monte de Caparica, 2829-511 Almada, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0167-4077","authenticated-orcid":false,"given":"Jos\u00e9 Jo\u00e3o","family":"Mendes","sequence":"additional","affiliation":[{"name":"Centro de Investiga\u00e7\u00e3o Interdisciplinar Egas Moniz (CiiEM), Instituto Universit\u00e1rio Egas Moniz (IUEM), Monte de Caparica, 2829-511 Almada, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8694-6459","authenticated-orcid":false,"given":"Marco M. M.","family":"Gresnigt","sequence":"additional","affiliation":[{"name":"University Medical Center Groningen, Department of Restorative Dentistry and Biomaterials, Center for Dentistry and Oral Hygiene, University of Groningen, 9713 AV Groningen, The Netherlands"},{"name":"Department of Special Dental Care, Martini Hospital, 9728 NT Groningen, The Netherlands"},{"name":"Faculty of Health Sciences, University Arthuro Prat, Iquique 2120, Chile"}]}],"member":"1968","published-online":{"date-parts":[[2022,3,10]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"2661","DOI":"10.1080\/01694243.2012.691038","article-title":"Adhesion concepts in dentistry: Tooth and material aspects","volume":"26","year":"2012","journal-title":"J. Adhes. Sci. Technol."},{"key":"ref_2","first-page":"18","article-title":"Ceramics overview: Classification by microstructure and processing methods","volume":"31","author":"Giordano","year":"2010","journal-title":"Compend. Contin. Educ. Dent."},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"109","DOI":"10.1007\/s12633-011-9078-7","article-title":"Insights on Ceramics as Dental Materials. Part I: Ceramic Material Types in Dentistry","volume":"3","author":"Ho","year":"2011","journal-title":"Silicon"},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1186\/s12903-019-0838-x","article-title":"Current status on lithium disilicate and zirconia: A narrative review","volume":"19","author":"Zarone","year":"2019","journal-title":"BMC Oral Health"},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"6","DOI":"10.1016\/S0022-3913(10)60086-8","article-title":"Translucency of zirconia copings made with different CAD\/CAM systems","volume":"104","author":"Baldissara","year":"2010","journal-title":"J. Prosthet. Dent."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"208","DOI":"10.1016\/j.jpor.2014.07.003","article-title":"Ceramic dental biomaterials and CAD\/CAM technology: State of the art","volume":"58","author":"Li","year":"2014","journal-title":"J. Prosthodont. Res."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"63","DOI":"10.1016\/j.dental.2017.08.031","article-title":"Flexural resistance of heat-pressed and CAD-CAM lithium disilicate with different translucencies","volume":"33","author":"Carrabba","year":"2017","journal-title":"Dent. Mater."},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"241","DOI":"10.2341\/13-291-S","article-title":"Digital Workflow for Virtually Designing and Milling Ceramic Lithium Disilicate Veneers: A Clinical Report","volume":"40","author":"Zandinejad","year":"2015","journal-title":"Oper. Dent."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"43","DOI":"10.1016\/j.prosdent.2016.09.031","article-title":"Randomized controlled within-subject evaluation of digital and conventional workflows for the fabrication of lithium disilicate single crowns. Part II: CAD-CAM versus conventional laboratory procedures","volume":"118","author":"Sailer","year":"2017","journal-title":"J. Prosthet. Dent."},{"key":"ref_10","first-page":"318","article-title":"Luting of inlays, onlays, and overlays with preheated restorative composite resin does not prevent seating accuracy","volume":"13","author":"Magne","year":"2018","journal-title":"Int. J. Esthet. Dent."},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"1351","DOI":"10.1016\/j.dental.2019.07.001","article-title":"Influence of bonding surface and bonding methods on the fracture resistance and survival rate of full-coverage occlusal veneers made from lithium disilicate ceramic after cyclic loading","volume":"35","author":"Krummel","year":"2019","journal-title":"Dent. Mater."},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"372","DOI":"10.2341\/14-116-L","article-title":"Influence of Etching Protocol and Silane Treatment with a Universal Adhesive on Lithium Disilicate Bond Strength","volume":"40","author":"Kalavacharla","year":"2015","journal-title":"Oper. Dent."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"17","DOI":"10.1186\/s40563-017-0096-6","article-title":"Post-etching cleaning influences the resin shear bond strength to CAD\/CAM lithium-disilicate ceramics","volume":"5","author":"Bruzi","year":"2017","journal-title":"Appl. Adhes. Sci."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"S50","DOI":"10.1080\/07853890.2021.1897360","article-title":"Influence of silane type and application time on the bond strength to leucite reinforced ceramics","volume":"53","author":"Rita","year":"2021","journal-title":"Ann. Med."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"606","DOI":"10.2341\/16-215-L","article-title":"Effect of Hydrofluoric Acid Concentration and Etching Time on Bond Strength to Lithium Disilicate Glass Ceramic","volume":"42","author":"Sundfeld","year":"2017","journal-title":"Oper. Dent."},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"492","DOI":"10.1590\/0103-6440201802080","article-title":"Adhesion to a Lithium Disilicate Glass Ceramic Etched with Hydrofluoric Acid at Distinct Concentrations","volume":"29","author":"Prochnow","year":"2018","journal-title":"Braz. Dent. J."},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"467","DOI":"10.1016\/j.dental.2012.02.009","article-title":"Aspects of silane coupling agents and surface conditioning in dentistry: An overview","volume":"28","author":"Lung","year":"2012","journal-title":"Dent. Mater."},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"13","DOI":"10.1016\/j.dental.2017.09.002","article-title":"Silane adhesion mechanism in dental applications and surface treatments: A review","volume":"34","author":"Matinlinna","year":"2018","journal-title":"Dent. Mater."},{"key":"ref_19","first-page":"579","article-title":"Dissolution Depth and Surface Morphological Alterations in Ultrathin Glass Ceramic Etched with Different Hydrofluoric Acid -etching Protocols","volume":"23","author":"Garfias","year":"2021","journal-title":"J. Adhes. Dent."},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"210","DOI":"10.2341\/17-355-L","article-title":"Does a Self-Etching Ceramic Primer Improve Bonding to Lithium Disilicate Ceramics? Bond Strengths and FESEM Analyses","volume":"44","author":"Lopes","year":"2018","journal-title":"Oper. Dent."},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"1082","DOI":"10.1016\/j.dental.2019.05.002","article-title":"Silane reactivity and resin bond strength to lithium disilicate ceramic surfaces","volume":"35","author":"Dimitriadi","year":"2019","journal-title":"Dent. Mater."},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"1411","DOI":"10.1016\/j.ceramint.2019.09.105","article-title":"Physicochemical surface characterizations of four dental CAD\/CAM lithium disilicate-based glass ceramics on HF etching: An XPS study","volume":"46","author":"Bebsh","year":"2020","journal-title":"Ceram. Int."},{"key":"ref_23","first-page":"203","article-title":"Effect of MDP-containing Silane and Adhesive Used Alone or in Combination on the Long-term Bond Strength and Chemical Interaction with Lithium Disilicate Ceramics","volume":"19","author":"Cardenas","year":"2017","journal-title":"J. Adhes. Dent."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"e95","DOI":"10.1016\/j.dental.2016.11.004","article-title":"Does 8-methacryloxyoctyl trimethoxy silane (8-MOTS) improve initial bond strength on lithium disilicate glass ceramic?","volume":"33","author":"Maruo","year":"2017","journal-title":"Dent. Mater."},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"834","DOI":"10.4012\/dmj.2013-153","article-title":"Composite resin vs resin cement for luting of indirect restorations: Comparison of solubility and shrinkage behavior","volume":"32","author":"Bortolotto","year":"2013","journal-title":"Dent. Mater. J."},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"4225","DOI":"10.1007\/s00784-020-03637-2","article-title":"Heating and preheating of dental restorative materials\u2014a systematic review","volume":"24","author":"Lopes","year":"2020","journal-title":"Clin. Oral Investig."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"133","DOI":"10.1016\/j.dental.2016.11.015","article-title":"Academy of Dental Materials guidance on in vitro testing of dental composite bonding effectiveness to dentin\/enamel using micro-tensile bond strength (\u03bcTBS) approach","volume":"33","author":"Armstrong","year":"2017","journal-title":"Dent. Mater."},{"key":"ref_28","doi-asserted-by":"crossref","unstructured":"Magne, P., Bruzi, G., Carvalho, A., Enciso, R., and Giannini, M. (2018). Optimization of Heat-Dried Silane Application for CAD\/CAM Ceramic Resin Bonding. Nanosci. Nanotechnol., 2.","DOI":"10.18063\/nn.v2i1.414"},{"key":"ref_29","doi-asserted-by":"crossref","unstructured":"Ramakrishnaiah, R., Alkheraif, A.A., Divakar, D.D., Matinlinna, J.P., and Vallittu, P.K. (2016). The Effect of Hydrofluoric Acid Etching Duration on the Surface Micromorphology, Roughness, and Wettability of Dental Ceramics. Int. J. Mol. Sci., 17.","DOI":"10.3390\/ijms17060822"},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"224","DOI":"10.1111\/j.1708-8240.2005.tb00119.x","article-title":"Surface treatment protocols in the cementation process of ceramic and laboratory-processed composite restorations: A literature review","volume":"17","author":"Soares","year":"2005","journal-title":"J. Esthet. Restor. Dent."},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"53","DOI":"10.1016\/S0300-5712(96)00078-4","article-title":"Effect of different etching periods on the bond strength of a composite resin to a machinable porcelain","volume":"26","author":"Chen","year":"1998","journal-title":"J. Dent."},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"1164","DOI":"10.1016\/j.prosdent.2014.04.021","article-title":"Influence of particle abrasion or hydrofluoric acid etching on lithium disilicate flexural strength","volume":"112","author":"Menees","year":"2014","journal-title":"J. Prosthet. Dent."},{"key":"ref_33","doi-asserted-by":"crossref","first-page":"832","DOI":"10.1016\/j.dental.2021.02.006","article-title":"Chemical surface modification of lithium disilicate needles of a silica-based ceramic after HF-etching and ultrasonic bath cleaning: Impact on the chemical bonding with silane","volume":"37","author":"Ogden","year":"2021","journal-title":"Dent. Mater."},{"key":"ref_34","first-page":"OP-21","article-title":"Silane coupling agent type and application time influences the bond strength of resin-feldspathic CAD\/CAM ceramics","volume":"44","author":"Delgado","year":"2019","journal-title":"Restor. Dent. Endod."},{"key":"ref_35","doi-asserted-by":"crossref","first-page":"340","DOI":"10.1016\/j.jpor.2019.01.008","article-title":"Bonding of different self-adhesive resins to high-strength composite resin block treated with surface conditioning","volume":"63","author":"Yu","year":"2019","journal-title":"J. Prosthodont. Res."},{"key":"ref_36","doi-asserted-by":"crossref","first-page":"104026","DOI":"10.1016\/j.jmbbm.2020.104026","article-title":"Effects of the ratio of silane to 10-methacryloyloxydecyl dihydrogenphosphate (MDP) in primer on bonding performance of silica-based and zirconia ceramics","volume":"112","author":"Koko","year":"2020","journal-title":"J. Mech. Behav. Biomed. Mater."},{"key":"ref_37","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1186\/s40563-018-0109-0","article-title":"Bonding of CAD\/CAM lithium disilicate restorations with regular and flowable composite resin with and without wetting resin","volume":"6","author":"Bruzi","year":"2018","journal-title":"Appl. Adhes. Sci."},{"key":"ref_38","doi-asserted-by":"crossref","unstructured":"Dimitriadi, M., Zinelis, S., Zafiropoulou, M., Silikas, N., and Eliades, G. (2020). Self-Etch Silane Primer: Reactivity and Bonding with a Lithium Disilicate Ceramic. Materials, 13.","DOI":"10.3390\/ma13030641"},{"key":"ref_39","doi-asserted-by":"crossref","first-page":"75","DOI":"10.1016\/j.jpor.2017.06.002","article-title":"Self-etching ceramic primer versus hydrofluoric acid etching: Etching efficacy and bonding performance","volume":"62","author":"Gaintantzopoulou","year":"2018","journal-title":"J. Prosthodont. Res."},{"key":"ref_40","first-page":"33","article-title":"Bond strength of resin cement to ceramic with simplified primers and pretreatment solutions-PubMed","volume":"66","author":"Swank","year":"2018","journal-title":"Gen. Dent."},{"key":"ref_41","first-page":"261","article-title":"Effect of Different Surface Treatments on the Tensile Bond Strength to Lithium Disilicate Glass Ceramics","volume":"20","author":"Lyann","year":"2018","journal-title":"J. Adhes. Dent."},{"key":"ref_42","first-page":"491","article-title":"Durability of Resin Bonding to Lithium Disilicate and Zirconia Ceramic using a Self-etching Primer","volume":"19","author":"Wille","year":"2017","journal-title":"J. Adhes. Dent."},{"key":"ref_43","first-page":"133","article-title":"Different Etching Times of a One-step Ceramic Primer: Effect on the Resin Bond Strength Durability to a CAD\/CAM Lithium-Disilicate Glass-Ceramic","volume":"23","author":"Dapieve","year":"2021","journal-title":"J. Adhes. Dent."},{"key":"ref_44","doi-asserted-by":"crossref","first-page":"259","DOI":"10.4047\/jap.2016.8.4.259","article-title":"Effect of surface treatments on shear bond strength of resin composite bonded to CAD\/CAM resin-ceramic hybrid materials","volume":"8","author":"Nemli","year":"2016","journal-title":"J. Adv. Prosthodont."},{"key":"ref_45","doi-asserted-by":"crossref","first-page":"809","DOI":"10.1016\/j.dental.2018.02.004","article-title":"Acidic pH weakens the bonding effectiveness of silane contained in universal adhesives","volume":"34","author":"Yao","year":"2018","journal-title":"Dent. Mater."},{"key":"ref_46","doi-asserted-by":"crossref","first-page":"413","DOI":"10.7569\/RAA.2014.097309","article-title":"Bonding Dissimilar Materials in Dentistry: A Critical Review","volume":"2","author":"Zakir","year":"2014","journal-title":"Rev. Adhes. Adhes."}],"container-title":["Materials"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1996-1944\/15\/6\/2045\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,10]],"date-time":"2025-10-10T22:34:23Z","timestamp":1760135663000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1996-1944\/15\/6\/2045"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2022,3,10]]},"references-count":46,"journal-issue":{"issue":"6","published-online":{"date-parts":[[2022,3]]}},"alternative-id":["ma15062045"],"URL":"https:\/\/doi.org\/10.3390\/ma15062045","relation":{},"ISSN":["1996-1944"],"issn-type":[{"type":"electronic","value":"1996-1944"}],"subject":[],"published":{"date-parts":[[2022,3,10]]}}}