Resumos em peri??dicos
New method for depth analysis of Y-TZP t-m phase transformation
Registro en:
0109-5641
33
suppl. 1
10.1016/j.dental.2017.08.009
Autor
ARATA, A.
PRETTO, L.R. de
USSUI, V.
LIMA, N.B.
FREITAS, A.Z.
MACHADO, J.P.B.
TANGO, R.N.
SOUZA, G.M. de
LAZAR, D.R.R.
Resumen
Purpose/aim: The aim of this studywas to validate the optical
coherence tomography (OCT) as a nondestructive method
of analysis to evaluate the depth of tetragonal to monoclinic
(t-m) transformed zone and to calculate the kinetics
of phase transformation of a monolithic Y-TZP after hydrothermal
aging. Specifically, to compare the activation energy
of t-m transformation calculated by the depth of the transformed
zone using scanning electron microscopy (SEM) and
OCT.
Materials and methods: Fully sintered (1450 ???C/2 h) discs of
dentalY-TZP (LAVAPLUS, 3M-ESPE)were aged in hydrothermal
pressurized reactor to follow the phase transformation kinetics
at 120 to 150 ???C. Four samples per aging time were
analyzed by OCT (OCP930SR, Thorlabs Inc.), = 930 nm, spectral
bandwidth (FWHM) of 100 nm, nominal resolution of
6 m (lateral and axial) in air, declared digital resolution
3.09 m (axial). Three areas of 3mm (lateral) were observed
to calculate the phase transformation depth (Image J).
X-ray diffraction analysis (XRD) were performed, Cu-K ,
20??? to 80???, 2 . The data were refined using the Rietveld
method (GSAS). The transversal section of one specimen
of each group was submitted to backscattered SEM analysis
to calculate the phase transformation depth (Image
J). The speed of the transformation zone front was determined
plotting the phase transformation depth versus aging
time.
Results: XRD results indicated that Y-TZP that 66% is the
maximum value of monoclinic phase concentration for all
aged Y-TZP. The activation energy for the monolithic Y-TZP
was 107.53 kJ/mol. One year and 5 years of hydrothermal aging
at 37 ???C will present approximately 4.21% and 15% of monoclinic
phase, respectively. The comparison of the depth of the
transformed zone using SEM and OCT were similar, showing
a linear behavior and providing information that the opaque
layer observed by OCT is related to the depth of the transformed
zone (Fig. 1), any difference among the results could
be a result of the refraction index correction. The energy of
activation calculated by SEM and OCT were 114 kJ/mol and
100 kJ/mol, respectively. The speed calculated for the phase
transformation into the bulk of the transformed zone estimated
for 37 ???C was 0.04 m/year (SEM) and 0.16 m/year
(OCT). Conclusions: The results indicate that activation energy
values determined by SEM and OCT observations were similar
allowing the use of the OCT as a tool for monolithic Y-TZP
t-m phase transformation kinetic evaluation. Moreover, OCT
method has the advantage of a shorter analysis time, without
the need of sample preparation steps.