Authors: Junji Ikeda, Megumi Mabuchi, Takefumi Nakanishi, Fumiaki Miyaji, Masaru Ueno, Giuseppe Pezzotti
Abstract: As for zirconia toughened alumina (ZTA) with various ratios of alumina/zirconia, crystal
and micro structures, fracture toughness and phase stability were evaluated by X-ray diffraction,
Raman spectroscopy, and aging test in hydrothermal environment. The grain size and monoclinic
fraction of zirconia phase and residual stress in alumina matrix changed as a function of zirconia
content. The ZTA showed higher fracture toughness than conventional alumina. The fracture
toughness of ZTA was highest at which the content of tetragonal zirconia was maximum. The
monoclinic fraction of ZTA did not increase even after aging test at 121°C for 150 hr. This study
indicates that the optimization of tetragonal zirconia content is essential for achieving higher
fracture toughness of ZTA. The ZTA with phase stability as well as with fracture toughness is
expected as bearing materials which could extend lifetime of artificial joints in clinical use.
767
Authors: Junji Ikeda, Fumiaki Miyaji, Masaru Ueno, Giuseppe Pezzotti
Abstract: Phase stability of 3 mol% yttria stabilized polycrystalline zirconia ceramics (3Y-TZP)
was evaluated by aging test in water vapor environment and Raman spectroscopic technique. In our
previous study, it has been confirmed that phase stability was improved by controlling sintering
temperature. In this study, we pointed our attention and evaluated the influence of surface
conditions related to machining and to heat treatment, thus monitoring the changes in phase
transformation fraction and residual stress on the material surface. From the results of aging test, an
increase in monoclinic fraction was observed for grinded surfaces as compared with polished
surfaces. Samples subjected to heat treatment after machining showed improved phase stability. A
Vickers indentation print was also introduced on a 3Y-TZP surface, and the relationship between
surface condition and low temperature aging was evaluated in the neighborhood of the print. We
found that the residual stress fields induced in phase-transformed areas were enhanced during low
temperature aging, and that phase stability was improved by heat treatment.
755
Authors: Takefumi Nakanishi, Megumi Sasaki, Junji Ikeda, Fumiaki Miyaji, Makoto Kondo
Abstract: The JMM-ZTA, a kind of zirconia-toughened alumina, is a bearing ceramic newly
developed for artificial joints. Although it has already been reported that mechanical strength and
fracture toughness are higher in the JMM-ZTA than in alumina, the stability of the JMM-ZTA has
not been studied in detail yet. In the present study, the stability of the JMM-ZTA with respect to
mechanical strength and crystalline phases was examined under hydrothermal environment, and
the results were compared with those of alumina. Both the 4-point bending strength and the
fraction of monoclinic zirconia unchanged even after the aging test at 121°C for 300 h. These
results indicate that the JMM-ZTA possesses quite excellent stability to be used as bearing
material of artificial joints.
1267
Authors: Junji Ikeda, Giuseppe Pezzotti, Mikio Iwamoto, Masaru Ueno
Abstract: The kinetics of tetragonal-to-monoclinic phase transformation (t→m transformation) in the
earlier generation zirconia femoral heads was evaluated by X-ray diffractometry, laser microscopy and
Raman microprobe spectroscopy. From previous results of hip-simulator study, it was confirmed that
phase transformation on the surface of zirconia femoral heads had little influence on wear rate of
UHMWPE sockets, and in some zirconia femoral heads, only a slight increase in monoclinic fraction
was observed during hip-simulator test. In this study, we suggest that the models of phase transformation
progress during tests in hip-simulator and aging tests are different based on both laser microscopic and
Raman/fluorescence spectroscopic observation. Besides this finding, this study shows that Raman
spectroscopy is a useful technique for the evaluation of the kinetics of phase transformation in femoral
heads after both in vitro and in vivo environmental exposure.
1203
Authors: Junji Ikeda, Giuseppe Pezzotti, Takefumi Nakanishi
Abstract: The phase stability under aqueous condition and changes in the wear region after the Pin-on-Flat wear testing were evaluated using Raman and fluorescence spectroscopy techniques and X-ray diffractometry for a newly
developed zirconia toughened alumina (JMM-ZTA). This study suggests that JMM-ZTA is a highly stable material under aqueous environment in the human body and has a high wear resistance in Pin-on-Flat wear tests. This results from a transformation toughening mechanism operative in JMM-ZTA. Therefore,
JMM-ZTA appears to have a possibility to improve the performance of monolithic alumina as a material for hip and knee joint prostheses.
1243
Authors: Masaru Ueno, Mikio Iwamoto, Junji Ikeda
Abstract: Several clinical reports pointed out that the monoclinic transformation of crystalline
structure of zirconia femoral head with clinical service time can cause the changes of surface roughness and mechanical properties. To elucidate the relationship between these surface roughness change induced by phase transformation and UHMWPE socket wear, hip simulator wear tests were performed on total hip prostheses (THP) up to 6 million cycles running. Four groups of different
surface monoclinic phase fraction of Kyocera zirconia heads were prepared by aging treatment prior to the wear tests. The surface roughness/ wear rate of zirconia heads with 0, 10, 50 and 80mol% monoclinic phase fraction were 0.009/ 3.8, 0.014/ 3.9, 0.012/ 3.7 and 0.010µmRa/ 3.1mg/million cycles, respectively. These results exhibit that the surface roughness change induced by phase
transformation does not significantly influence extent of the generation of UHMWPE debris in Kyocera zirconia /UHMWPE THP system. In contrast, the surface roughness exhibited complex relation with the monoclinic phase fraction and therefore the morphological analysis was performed on the zirconia articulating surfaces
1239
Authors: Junji Ikeda, Giuseppe Pezzotti, Makoto Kondo
Abstract: Phase stability of 3Y-TZP was evaluated by acceleration test in water vapor environment and Raman spectroscopy. We found that the phase stability was affected not only by grain size but also by residual stress field, which could be quantitatively measured by Raman piezo-spectroscopy
and controlled by sintering temperature. This study shows that Raman spectroscopy is a very useful technique for non-destructive analysis of 3Y-TZP.
1227
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.
1215
Authors: Giuseppe Pezzotti, Ian C. Clarke, C. Jobe, T. Donaldson, Kengo Yamamoto, Toshiyuki Tateiwa, T. Kumakura, R. Tsukamoto, Junji Ikeda
Abstract: A survey of confocal Raman/fluorescence microprobe spectroscopic techniques is presented with emphasis placed on surface analysis of artificial hip joints. Suitable instrumental configurations are first explained in
some details in order to describe the versatility of the spectroscopic microprobes to biomedical materials analyses. Then, these notions, which represent the foundation for structural and mechanical analyses of joint surfaces, are applied to selected cases of paramount importance in hip arthroplasty.
1211
Authors: Takayoshi Shimozono, Junji Ikeda, Giuseppe Pezzotti
Abstract: Structural reliability, biocompatibility and bioinertness are fundamental prerequisites for bioceramics used in artificial hip and knee joints. Among structural properties, superior fracture toughness is necessary for guaranteeing high reliability during implantation lifetime. Bioinert ceramics employed in artificial joints are mainly limited to alumina and zirconia materials. In this paper, the critical crack-tip stress intensity factor, KI0, and the tetragonal-to-monoclinic phase-transformation behavior of a 3 mol % Y2O3-doped tetragonal ZrO2 polycrystals (3Y-TZP)
were studied as a function of grain size. 3Y-TZP’s with four different grain sizes were prepared and the size and morphology of the monoclinic transformation zone generated around the tip of an indentation crack were analyzed by quantitative Raman microprobe spectroscopy. The stress intensity factor, KI0, was evaluated by the crack opening displacement (COD) method using a recently proposed equation for calculating the compliance of an indentation crack.
1207