RESUMEN
We propose the use of Optical Coherence Tomography (OCT) as a tool for the quality control of 3-D-printed ceramics. Test samples with premeditated defects, namely single- and two-component samples of zirconia, titania, and titanium suboxides, were printed by stereolithography-based DLP (Digital Light Processing) processes. The OCT tomograms obtained on the green samples showed the capability of the method to visualize variations in the layered structure of the samples as well as the presence of cracks and inclusions at depths up to 130 µm, as validated by SEM images. The structural information was visible in cross-sectional images as well as in plan-view images. The optical signal measured from the printed zirconia oxide and titanium oxide samples showed strong attenuation with depth and could be fit with an exponential decay curve. The variations of the decay parameter correlated very well with the presence of defects and material variation. When used as an imaging quantity, the decay parameter projects the position of the defects into 2-D (X,Y) coordinates. This procedure can be used in real time, it reduces the data volume up to 1000 times, and allows for faster subsequent data analysis and transfer. Tomograms were also obtained on sintered samples. The results showed that the method can detect changes in the optical properties of the green ceramics caused by sintering. Specifically, the zirconium oxide samples became more transparent to the light used, whereas the titanium suboxide samples became entirely opaque. In addition, the optical response of the sintered zirconium oxide showed variations within the imaged volume, indicating material density variations. The results presented in this study show that OCT provides sufficient structural information on 3-D-printed ceramics and can be used as an in-line tool for quality control.
RESUMEN
Stiffness-load curves obtained in quantitative atomic force acoustic microscopy (AFAM) measurements depend on both the elastic properties of the sample and the geometry of the atomic force microscope (AFM) tip. The geometry of silicon AFM tips changes when used in contact mode, affecting measurement accuracy. To study the influence of tip geometry, we subjected ten AFM tips to the same series of AFAM measurements. Changes in tip shape were observed in the scanning electron microscope (SEM) between individual AFAM tests. Because all of the AFAM measurements were performed on the same sample, variations in AFAM stiffness-load curves were attributed to differences in tip geometry. Contact-mechanics models that assumed simple tip geometries were used to analyze the AFAM data, but the calculated values for tip dimensions did not agree with those provided by SEM images. Therefore, we used a power-law approach that allows for a nonspherical tip geometry. We found that after several AFAM measurements, the geometry of the tips at the very end is intermediate between those of a flat punch and a hemisphere. These results indicate that the nanoscale tip-sample contact cannot easily be described in terms of simple, ideal geometries.