Authors: Kiyotaka Yamada, Masahiro Nawa, Giuseppe Pezzotti
Abstract: In the area of dental treatment for crown and dental implants, ceramics restoration is
becoming popular due to both aesthetic needs and release of metallic allergy. However, for the
restoration of defected tooth, ceramics materials with higher reliability than that of conventional
glass or alumina have been required, thus raising expectations for zirconia ceramics. Since residual
stress play a significant role in the reliability of dental implants, in this paper, a non-destructive
assessment of residual stress is presented for a zirconia-substrate/VINTAGE ZR T-Glass system
using confocal fluorescence microprobe spectroscopy.
821
Authors: Masahiro Nawa, Kiyotaka Yamada, Giuseppe Pezzotti
Abstract: With elongation of average human life, problem such as bone embrittlement and
osteoporosis call for quick solution and the expectation for artificial biomaterials heightens. Many
ceramics widely used as artificial biomaterials are limited by their poor reliability characteristics. A
CeO2 stabilized tetragonal zirconia polycrystalline (Ce-TZP) matrix incorporating nanometer sized
Al2O3 particles within the zirconia grains (Ce-TZP/Al2O3) was recently developed. This material
experienced significant improvements in both fracture toughness and strength above the standard
mechanical performance of monolithic zirconia. In this paper, we performed a macro/microscopic
fracture mechanics assessment of this developed Ce-TZP/Al2O3 nanocomposite, in comparison with
a 3 mol% Y-TZP according to advanced in situ confocal Raman spectroscopy techniques.
813
Authors: Kiyotaka Yamada, Giuseppe Pezzotti
Abstract: Alumina matrix composite (AMC) has been widely used for artificial hip and knee joints
because of its phase stability in human body and its excellent wear resistance. The excellent
mechanical properties of strength and fracture toughness of zirconia materials are well known to be
closely related to stress-induced transformation from the tetragonal to the monoclinic phase, which
is accompanied with 4% volume increase of the zirconia crystal cell. However, it is also to be
considered that the material is prone to low temperature aging degradation (LTAD) under
hydrothermal environment, like in the human body. This LTAD is influenced by the tetragonal to
the monoclinic (t-m) phase transformation. T-m transformation also induces the formation of
microcracks at the material surface, and an increase in surface. Microcracking leads to a decrease of
mechanical properties, and could explain the failure of implants after some years in vivo [1, 2]
.Therefore, it is very important to study how to prevent phase transformation in zirconia
components. Transformed monoclinic zirconia percentage can be experimentally measured by
Raman spectroscopy and the residual stress distribution, which is related to phase transformation,
can be determined by a non-destructive piezo-spectroscopic analysis. In this paper, we attempted to
evaluate it from both stress and mechanical properties points of view by confocal Raman and
fluorescence spectroscopy.
783
Authors: Kiyotaka Yamada, Masahiro Nawa, Giuseppe Pezzotti
Abstract: Zirconia ceramics have been widely used for new generation of bearing materials in
biomedical applications. In this context, a zirconia-matrix, stabilized with cerium oxide and
dispersed with fine alumina particles (Ce-TZP/Al2O3 nanocomposite) was recently developed and
this material experienced significant improvements in both fracture toughness and strength above
the standard mechanical performance of monolithic zirconia. In this paper, we used confocal Raman
spectroscopy to provide quantitative assessments with high spatial resolution of phase structure and
residual stress fields developed in the Ce-TZP/Al2O3 nanocomposite. According to confocal Raman
spectroscopy, we have directly visualized patterns of phase transformation and residual stress fields
stored on the very surface of the material around an indentation print. These spectroscopic
assessments may open a perspective in understanding the micromechanical behavior of the
Ce-TZP/Al2O3 nanocomposite when subjected to local surface impingement and shocks.
373
Authors: Giuseppe Pezzotti, Kiyotaka Yamada, S. Shiroyama, Masahiro Nawa
Abstract: Zirconia ceramics were introduced in the seventhies for use as structural biomaterials after
laboratory tests and simulator studies. However, nowadays concerns remain about their reliability in
vivo, despite published clinical studies have already established the safety and the good tribological
performance of these materials. It is still unclear what level of reliability can be achieved in ceramic
biomaterials and how much their toughness level can be enhanced by microstructural design. The
polycrystalline nature of ceramic materials may make both the observed properties and performance
very scattered. In particular, the grain size and other microstructural features likely play a fundamental
role in the mechanical behavior of the material. In this paper, we propose a set of fracture mechanics
assessments, aimed to establish the quantitative amount of toughness achievable in a zirconia/alumina
nanocomposite stabilized with cerium oxide (Ce-TZP/Al2O3 nanocomposite), and in situ confocal
Raman spectroscopy to visualize toughening mechanisms, including polymorph transformation and
residual stress fields stored around the crack path.
337
Authors: Giuseppe Pezzotti, Andrea Leto, Kiyotaka Yamada, Alessandro Alan Porporati
Abstract: Electro-stimulated piezo-spectroscopy (PS) can be quantitatively used for obtaining
information about applied and residual stress fields piled up in ceramic materials and devices. PS
experiments can be conducted in a field-emission-gun scanning electron microscope (FEG-SEM)
equipped with a high spectral resolution cathodoluminescence (CL) spectrometer. Micromechanical
information can be thus added to the microscopic crystallographic and chemical information already
available in conventional SEM devices. Independent of the physical mechanisms behind CL
emission, the spectral position of selected bands in ceramics is shown to possess high stress
sensitivity. In addition, given the high scanning flexibility and spatial resolution of the electron
beam, residual stress assessments can be performed on relatively large areas with significantly
improved spatial resolution as compared with the more popular photo-stimulated PS approach (i.e.,
using a laser beam as the excitation source). In this paper, we first quantitatively characterize the
stress dependence of the spectroscopic bands observed in ruby. Then, based on this knowledge, an
application is shown of bi-dimensional residual stress mapping around an indentation print.
1658
Authors: Kiyotaka Yamada, Junji Ikeda, Giuseppe Pezzotti
Abstract: The electro-stimulated luminescence spectrum of a rare-earth ion added to zirconia
(ZrO2) lattice was investigated with the aim of using it as a sensor for nano-scale stress (fluorescence piezo-spectroscopy) and phase transformation assessments in a field emission scanning electron microscope (FE-SEM). In this paper, the selected rare-earth fluorescent ion Eu, added to ZrO2 as a raw oxide powder (Eu2O3) before sintering (in the amount of 1.0 wt. %).
Spectroscopic results indicated that the spectral shift of some fluorescent band of the selected rare-earth ion was sensitive to residual stress and that the electron-stimulated spectra of Eu2O3-doped ZrO2 in its tetragonal and monoclinic polymorphs were different to each other. Based on these findings, the luminescent substance can be useful as a “stress and phase transformation
sensor”, in order to clarify the elementary mechanisms behind synthetic ZrO2.
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