Calibration Curve for Quantitative Analysis of the Monoclinic-Tetragonal ZrO<sub>2</sub>System by X-Ray Diffraction

Toraya, Hideo; Yoshimura, Masahiro; Sōmiya, Shigeyuki

doi:10.1111/j.1151-2916.1984.tb19715.x

Cited by 657 publications

(457 citation statements)

References 12 publications

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“…The phase analysis was conducted (n = 2) using an X-ray diffractometer (2θ range of 25 to 35 degrees; scan time of 1 sec/step, at 40 kV, 40 mA, step size of 0.03°; Bruker AXS, D8 Advance, Karlsruhe, Germany), through the Garvie & Nicholson method modified by Toraya and collaborators, 17 to determine the amount of m-phase content observed after each aging condition. This method has been extensively used 8 and described in the literature.…”

Section: Phase Transformation Analysismentioning

confidence: 99%

Mechanical behavior of yttria-stabilized tetragonal zirconia polycrystal: Effects of different aging regimens

et al. 2017

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This study aimed to characterize and compare the effect of different aging regimens on surface characteristic (topography and roughness), structural stability (phase transformation) and mechanical performance (Weibull analysis) of a Y-TZP ceramic. Discs (15 × 1.2 mm; VITA In-Ceram YZ) were prepared according to ISO 6872-2015 for biaxial flexural strength testing and randomly assigned into five groups (n = 30): as-sintered, no aging treatment (CTRL); 20 h in autoclave at 134°C, 2 bar pressure (AUT); intermittent mechanical loading at 20 Hz/10 6 load pulses (MechLoad); AUT followed by MechLoad (AUT+MechLoad); and storage in distilled water at 37°C, for 1 year (STO). The following analyses were performed: roughness (n = 30), surface topography (n = 2), phase transformation (n = 2) and biaxial flexure strength (n = 30). Phase transformation (increase of m-phase content) was shown to be a spontaneous, unavoidable and time-dependent process, occurring even under ambient conditions (dry storage after 1 year = 6.0% increase), and is considerably accelerated in the presence of moisture (STO = 17.6%; AUT= 63.1%; and AUT+MechLoad = 59.9%). For roughness parameters, only Ra was affected by aging, and the highest values were observed for AUT+MechLoad (0.25 ± 0.07 µm). For Weibull analysis, structural reliability (Weibull moduli) and characteristic strength were not impaired after aging, and some aging conditions led to increased values (highest weibull moduli in AUT, and highest characteristic strength in STO). Phase transformation proves to be a time-dependent spontaneous mechanism that is accelerated in the presence of different stimuli. However, none of the aging regimens had a negative effect on the characteristic strength and structural reliability of Y-TZP ceramic.

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Section: Phase Transformation Analysismentioning

confidence: 99%

Mechanical behavior of yttria-stabilized tetragonal zirconia polycrystal: Effects of different aging regimens

et al. 2017

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“…After the treatment, the monoclinic phase volume fraction (Vm%) near the surface was measured with XRD by applying the equation of Toraya et al (Toraya et al, 1984) and results were analyzed as in the previous section. This is a good indicator of the proneness of the material towards hydrothermal degradation.…”

Section: Aging Studiesmentioning

confidence: 99%

Surface roughened zirconia: towards hydrothermal stability

Camposilvan

Flamant

Anglada

2015

Journal of the Mechanical Behavior of Biomedical Materials

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Surface roughness is needed in several yttria-stabilized zirconia components used in restorative dentistry for osseointegration or adhesion purposes. This can be achieved by different treatments, which may also modify the microstructure of the surface. Among them, sandblasting and chemical etching are widely used, but their effect on hydrothermal aging of zirconia is not fully understood. In the present work, the zirconia long-term stability of rough surfaces prepared by these techniques is analyzed and a method is proposed for preventing hydrothermal aging while maintaining the original surface appearance and mechanical properties. The method involves pressure infiltration of a Cerium salt solution on the roughened surfaces followed by a thermal treatment. The solution, trapped by surface defects and small pores, is decomposed during thermal treatment into Cerium oxide, which is diffused at high temperature, obtaining Ce co-doping in the near-surface region.In addition, the microstructural changes induced in the near-surface by sandblasting or chemical etching are removed by the thermal treatment together with surface defects. No color modification was observed and the final roughness parameters were in the range of existing implants of proved good osseointegration. The aging resistance of Ce co-doped materials was strongly enhanced, showing the absence of aging after artificial degradation, increasing in this way the surface mechanical integrity.The proposed treatment is easily applicable to the current manufacturing procedures of zirconia dental posts, abutments, crowns and dentures, representing a solution to hydrothermal aging in these and other biomedical applications.

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“…The amount of monoclinic phase was determined from the X-Ray powder pattern fitting technique, using model proposed by Toraya et al 12 for ZrO 2 (Y 2 O 3 ) samples: The monoclinic phase fraction (X M ) was estimated in integrated intensity ration between ( 1 11) M and (111) M monoclinic phase peaks, and the (101) T tetragonal peak, according to Equation (1).…”

Section: Phase Analysismentioning

confidence: 99%

“…The volumetric fraction (V M ) of the monoclinic phase was then calculated by Equation (2) which is based on crystallographic correlations studied by Toraya et al 12 .…”

Section: Phase Analysismentioning

confidence: 99%

Recovery of Tetragonal Phase from Previously Transformed Y-TZP

et al. 2016

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ZrO 2 (Y 2 O 3 )-based ceramics are widely used as biomaterials due to high fracture toughness, resulting from the tetragonal-monoclinic phase transformation in which the ceramic is submitted during crack propagation. In this context, studies involving the possibility of optimization of the tetragonal phase are important for the properties improvement of this ceramic. This study investigated the recovery of tetragonal phase from a previously transformed ZrO 2 (3 mol% Y 2 O 3 ) ceramic. Zirconia samples were sintered at 1450 °C, at 1530 °C -2 h and at 1600 °C -4 h, in order to obtain materials with distinct microstructural features. The sintered samples were characterized by relative density, X-ray diffraction and scanning electron microscopy. Samples sintered at 1450 °C, 1530 °C -2 h and 1600 °C -4 h, presented relative densities of 94.2, 99.6 and 99.7% with grains size averages of 0.28, 0.49 and 1.31 μm, respectively. All samples were submitted to milling to induce the tetragonal→monoclinic phase transformation presenting 5, 50 and 65 vol% of monoclinic phase. Subsequently, heat treatments between 400 °C and 1200 °C were conducted to retransform monoclinic in tetragonal phase. It has been found that the smaller the grain size after sintering, the lower the necessary annealing temperatures for fully recovering of tetragonal phase. Annealing temperatures of 950, 1100 and 1200 °C were sufficient to recover almost fully the tetragonal phase.

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Calibration Curve for Quantitative Analysis of the Monoclinic-Tetragonal ZrO₂System by X-Ray Diffraction

Cited by 657 publications

References 12 publications

Mechanical behavior of yttria-stabilized tetragonal zirconia polycrystal: Effects of different aging regimens

Mechanical behavior of yttria-stabilized tetragonal zirconia polycrystal: Effects of different aging regimens

Surface roughened zirconia: towards hydrothermal stability

Recovery of Tetragonal Phase from Previously Transformed Y-TZP

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Calibration Curve for Quantitative Analysis of the Monoclinic-Tetragonal ZrO2System by X-Ray Diffraction

Cited by 657 publications

References 12 publications

Mechanical behavior of yttria-stabilized tetragonal zirconia polycrystal: Effects of different aging regimens

Mechanical behavior of yttria-stabilized tetragonal zirconia polycrystal: Effects of different aging regimens

Surface roughened zirconia: towards hydrothermal stability

Recovery of Tetragonal Phase from Previously Transformed Y-TZP

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Calibration Curve for Quantitative Analysis of the Monoclinic-Tetragonal ZrO₂System by X-Ray Diffraction