FIB/SEM and SEM/EDS microstructural analysis of metal-ceramic and zirconia-ceramic interfaces

Authors

  • F Massimi Universita di Roma
  • G Merlati Universita di Pavia
  • M Sebastiani Universita di Roma
  • P Battaini 38853 S.p.A
  • P Menghini Universita di Pavia
  • E Bemporad Universita di Roma

Abstract

Recently introduced FIB/SEM analysis in microscopy seems to provide a high-resolution characterization of the samples by 3D (FIB) cross-sectioning and (SEM) high resolution imaging. The aim of this study was to apply the FIB/SEM and SEM/EDS analysis to the interfaces of a metal-ceramic vs. two zirconiaceramic systems. Plate samples of three different prosthetic systems were prepared in the dental lab following the manufacturers’ instructions, where metal-ceramic was the result of a ceramic veneering (porcelain-fused-tometal) and the two zirconia- ceramic systems were produced by the dedicated CAD-CAM procedures of the zirconia cores (both with final sintering) and then veneered by layered or heat pressed ceramics. In a FIB/SEM equipment (also called DualBeam), a thin layer of platinum (1μm) was deposited on samples surface crossing the interfaces, in order to protect them during milling. Then, increasingly deeper trenches were milled by a focused ion beam, first using a relatively higher and later using a lower ion current (from 9 nA to 0.28 nA, 30KV). Finally, FEG-SEM (5KV) micrographs (1000–50,000X) were acquired. In a SEM the analysis of the morphology and internal microstructure was performed by 13KV secondary and backscattered electrons signals (in all the samples). The compositional maps were then performed by EDS probe only in the metal-ceramic system (20kV). Despite the presence of many voids in all the ceramic layers, it was possible to identify: (1) the grain structures of the metallic and zirconia substrates, (2) the thin oxide layer at the metalceramic interface and its interactions with the first ceramic layer (wash technique), (3) the roughness of the two different zirconia cores and their interactions with the ceramic interface, where the presence of zirconia grains in the ceramic layer was reported in two system possibly due to sandblasting before ceramic firing.

Author Biographies

F Massimi, Universita di Roma

University of Rome “ROMA TRE”, Mechanical and Industrial Engineering Department

G Merlati, Universita di Pavia

University of Pavia, Department of Odontostomatology, Dental Materials Unit

P Battaini, 38853 S.p.A

38853 S.p.A, Pero (MI), Italy

P Menghini, Universita di Pavia

University of Pavia, Department of Odontostomatology, Dental Materials Unit

E Bemporad, Universita di Roma

University of Rome “ROMA TRE”, Mechanical and Industrial Engineering Department

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Published

2012-01-10

Issue

Vol. 50 No. 3 (2011)

Section

Original Research Articles

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1. Conceived, planned, and performed the work leading to the report, or interpreted the evidence presented, or both;

2. Written the report or reviewed successive versions and shared in their revisions; and

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Further, I certify that:

1. This work has not been published elsewhere and is not under revision in another journal;

2. Humane procedures have been followed in the treatment of experimental animals (if applicable);

3. Investigations in humans was done in accordance with the ethical standards of the responsible committee on human experimentation or with the Helsinki Declaration (if applicable).

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5. The copyright of the article is transferred from the authors to the Bulletin du Groupement International pour la Recherche Scientifique en Stomatologie et Odontologie upon acceptance of the manuscript.