J Adv Prosthodont.  2016 Dec;8(6):479-488. 10.4047/jap.2016.8.6.479.

Interfacial modulus mapping of layered dental ceramics using nanoindentation

• Theocharopoulos AL
• Bushby AJ
• P'ng KM
• Wilson RM
• Tanner KE
• Cattell MJ

• KMID: 2382594
• DOI: http://doi.org/10.4047/jap.2016.8.6.479

Abstract

PURPOSE
The aim of this study was to test the modulus of elasticity (E) across the interfaces of yttria stabilized zirconia (YTZP) / veneer multilayers using nanoindentation.
MATERIALS AND METHODS
YTZP core material (KaVo-Everest, Germany) specimens were either coated with a liner (IPS e.max ZirLiner, Ivoclar-Vivadent) (Type-1) or left as-sintered (Type-2) and subsequently veneered with a pressable glass-ceramic (IPS e.max ZirPress, Ivoclar-Vivadent). A 5 µm (nominal tip diameter) spherical indenter was used with a UMIS CSIRO 2000 (ASI, Canberra, Australia) nanoindenter system to test E across the exposed and polished interfaces of both specimen types. The multiple point load - partial unload method was used for E determination. All materials used were characterized using Scanning Electron Microscopy (SEM) and X - ray powder diffraction (XRD). E mappings of the areas tested were produced from the nanoindentation data.
RESULTS
A significantly (P<.05) lower E value between Type-1 and Type-2 specimens at a distance of 40 µm in the veneer material was associated with the liner. XRD and SEM characterization of the zirconia sample showed a fine grained bulk tetragonal phase. IPS e-max ZirPress and IPS e-max ZirLiner materials were characterized as amorphous.
CONCLUSION
The liner between the YTZP core and the heat pressed veneer may act as a weak link in this dental multilayer due to its significantly (P<.05) lower E. The present study has shown nanoindentation using spherical indentation and the multiple point load - partial unload method to be reliable predictors of E and useful evaluation tools for layered dental ceramic interfaces.

Keyword

Elastic modulus; Fluorapatite; Zirconia

MeSH Terms

Ceramics*
Elastic Modulus
Hot Temperature
Methods
Microscopy, Electron, Scanning
Powder Diffraction

Figure

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  Fig. 1 Schematics of the indentation sites for the: preliminary testing (A) and final testing (B) of a Type-1 specimen. Type-2 had the same sites tested, but no interlayer was present.

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  Fig. 2 E versus depth of penetration graphs for Type-1 preliminary testing at: 10 mN (A), 30 mN (B) and 50 mN (C).

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  Fig. 3 E mappings across the interfaces of: (A) the Type-1 specimen (interlayer) and (B) the Type-2 specimen (no interlayer). The arrow indicates the lower modulus in the interlayer area.

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  Fig. 4 Nanoindentations on the Type-1 specimen (scale bar = 40 µm).

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  Fig. 5 SEM photomicrographs of: (A) KaVo Everest zirconia specimen showing fine grained crystal structure (scale bar = 1 µm), (B) IPS e.max ZirPress specimen showing fine nano-scale fibres in glassy matrix (scale bar = 1 µm), (C) IPS e.max ZirPress specimen showing a larger micro-particulate (scale bar = 1 µm), (D) IPS e.max ZirLiner specimen showing sparse nano-fibres in the glassy matrix (scale bar = 1 µm).

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  Fig. 6 X-ray diffraction patterns of: (a) KaVo Everest zirconia specimen showing a bulk tetragonal zirconia phase, (b) IPS e.max ZirPress specimen showing an amorphous profile, (c) IPS e.max ZirLiner specimen showing an amorphous profile.

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