Development and testing of multi-phase glazes for adhesive bonding to zirconia substrates

Polyxeni Ntala, Xiaohui Chen, Jason Niggli, Michael Cattell

    Research output: Contribution to journalArticlepeer-review


    Objectives: The aims of the study were to develop and test multi-phase glaze coatings for zirconia restorations, so that the surface could be etched and adhesively bonded. Methods: Zirconia disc specimens (n = 125, 16 mm × 1 mm) were cut from cylinders of Y-TZP (yttria-stabilized tetragonal zirconia polycrystals) ZS-Blanks (Kavo, Everest) and sintered overnight. Specimens were subjected to the recommended firing cycles, and next sandblasted. The specimens were divided into 5 groups of 25, with Group 1 as the sandblasted control. Groups 2-5 were coated with overglaze materials (P25 and IPS e.max Ceram glazes) containing secondary phases. Group 2 was (wt%): 10% hydroxyapatite (HA)/P25 glaze, Group 3: 20% IPS Empress 2 glass-ceramic/glaze, Group 4: 20% IPS Empress 2 glass/glaze and Group 5: 30% IPS Empress 2 glass/glaze. After sintering and etching, Monobond-S and composite resin cylinders (Variolink II, Ivoclar-Vivadent) were applied and light cured on the test surfaces. Specimens were water stored for 7 days. Groups were tested using the shear bond strength (SBS) test at a crosshead speed of 0.5 mm/min. Overglazed and the fractured specimen surfaces were viewed using secondary electron microscopy. Room and high temperature XRD and DSC were carried out to characterize the materials. Results: The mean (SD) SBS (MPa) of the test groups were: Group 1: 7.7 (3.2); Group 2: 5.6 (1.7); Group 3: 11.0 (3.0); Group 4: 8.8 (2.6) and Group 5: 9.1 (2.6). Group 3 was significantly different to the control Group 1 (p <0.05). There was no significant difference in the mean SBS values between Group 1 and Groups 2, 4 and 5 (p > 0.05). Group 2 showed statistically lower SBS than Groups 3-5 (p <0.05). Lithium disilicate fibres were present in Groups 3-5 and fine scale fibres were grown in the glaze following a porcelain firing cycle (Groups 4 and 5). XRD indicated a lithium disilicate/minor lithium orthophosphate phase (Group 3), and a tetragonal zirconia phase for the sintered Y-TZP ZS-Blanks. DSC and high temperature XRD confirmed the crystallization temperatures and phases for the IPS Empress 2 glass. Conclusions: The application of a novel glass-ceramic/glaze material containing a major lithium disilicate phase might be a step in improving the bond strength of a zirconia substrate to a resin cement. © 2010 Elsevier Ltd. All rights reserved.
    Original languageEnglish
    Pages (from-to)773-781
    Number of pages8
    JournalJournal of Dentistry
    Issue number10
    Publication statusPublished - Oct 2010


    • Adhesive bonding
    • Glaze
    • Microscopy
    • X-ray diffraction
    • Zirconia


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