Exfoliation of titanium nitride using a non-thermal plasma process.

In this study, we present a novel approach for the exfoliation of titanium nitride (TiN) powders utilizing a rapid, facile, and environmentally friendly non-thermal plasma method. This method involves the use of an electric arc and nitrogen as the ambient gas at room temperature to generate ionized particles. These ionized species interact with the ceramic crystal of TiN, resulting in a pronounced structural expansion. The exfoliated TiN products were comprehensively characterized using transmission electron microscopy, X-ray diffraction, and Raman spectroscopy. Remarkably, the cubic crystal structure of TiN was effectively retained, while the (200) crystal plane d-spacing increased from 2.08 to 3.09 Å, accompanied by a reduction in crystallite size and alterations in Raman vibrational modes. Collectively, these findings provide compelling evidence for the successful exfoliation of TiN structures using our innovative non-thermal plasma method, opening up exciting possibilities for advanced material applications.

Dental zirconia microwave-sintering followed by rapid cooling protocol.

OBJECTIVES: This study aimed to evaluate the effect of microwave sintering temperature and cooling rate (MS) on 3Y-TZP ceramics and its influence on the ceramic microstructure and mechanical properties. Specifically, to optimize the sintering process, reducing the total sintering time compared to conventional sintering. MATERIALS AND METHODS: Eighty-four pre-sintered Y-TZP discs (Vipi block Zirconn, VIPI) (ISO 6872) were divided into seven groups (n = 12) according to the sintering conditions: conventional sintering (CS) at 1530 °C for 120 min and microwave sintering at 1400 °C (MS1400) and 1450 °C (MS1450) for 15 min followed by different cooling conditions: rapid cooling (RC), cooling at 400 °C (C400) and 25 °C (C25). The specimens were submitted to apparent density measurements, X-ray diffraction analysis (XRD), scanning electron microscopy, and biaxial flexural strength test. Data was statistically analyzed through two-way ANOVA, Tukey, Sidak, Dunnett and Weibull (α = 0.05). RESULTS: All MS1400 groups presented lower density values than the CS and MS1450 groups. Two-way ANOVA revealed that the MS temperature and cooling rate affected the biaxial flexural strength of the Y-TZP (p < 0.01). Group MS1400RC presented lower biaxial flexural strength values (681.9 MPa) than MS1450RC (824.7 MPa). The cooling rate did not statistically decrease the biaxial strength among the groups submitted to microwave sintering at 1450 °C. XRD analysis showed that the sintering and cooling temperature did not induce tetragonal to monoclinic phase transformation. CONCLUSIONS: Microwave sintering at 1450 °C for 15 min followed by rapid cooling can be a viable fast alternative protocol for Y-TZP sintering, compared with the conventional sintering, reducing the total sintering time by 75% and reducing the energy used for the sintering process without affecting the Y-TZP biaxial flexural strength and relative density compared to the conventional sintering. Moreover, the microwave technique promoted smaller grains and did not induce monoclinic phase formation.

Development of Y-TZP/MWCNT-SiO2 nanocomposite for dental protheses.

Y-TZP/MWCNT-SiO2 nanocomposite was synthesized by co-precipitation and hydrothermal treatment methods. After the characterization of the MWCNT-SiO2 powder, specimens were obtained from the synthesized material Y-TZP/MWCNT-SiO2 by uniaxial pressing for a second characterization and later comparison of its optical and mechanical properties with the conventional Y-TZP. The MWCNT-SiO2 was presented in bundles of carbon nanotubes coated by silica (mean length: 5.10 ± 1.34 µm /D90: 6.9 µm). The composite manufactured was opaque (contrast ratio: 0.9929 ± 0.0012) and had a white color with a slightly difference from the conventional Y-TZP (ΔE00: 4.4 ± 2.2) color. The mechanical properties of Y-TZP/MWCNT-SiO2: vickers hardness (10.14 ± 1.27 GPa; p = 0.25) and fracture toughness (4.98 ± 0.30 MPa m1/2; p = 0.39), showed no significant difference from the conventional Y-TZP (hardness: 8.87 ± 0.89; fracture toughness: 4.98 ± 0.30 MPa m1/2). However, for flexural strength (p = 0.003), a lower value was obtained for Y-TZP/MWCNT-SiO2 (299.4 ± 30.5 MPa) when compared to the control Y-TZP (623.7 ± 108.8 MPa). The manufactured Y-TZP/MWCNT-SiO2 composite presented satisfactory optical properties, however the co-precipitation and hydrothermal treatment methods need to be optimized to avoid the formation of porosities and strong agglomerates, both from Y-TZP particles and MWCNT-SiO2 bundles, which lead to a significant decrease in the material flexural strength.

Effect of titania content and biomimetic coating on the mechanical properties of the Y-TZP/TiO2 composite.

OBJECTIVE: To investigate the effect of titania addition (0, 10 and 30mol%) on the microstructure, relative density, Young's modulus (E), Poisson's ratio (υ), mechanical properties (flexural strength, σf, and Weibull modulus, m) of a Y-TZP/TiO2 composite. The effect of the presence of a biomimetic coating on the microstructure and mechanical properties was also evaluated. METHODS: Y-TZP (3mol% of yttria) and Y-TZP/TiO2 composite (10 or 30mol% of titania) were synthesized by co-precipitation. The powders were pressed and sintered at 1400°C/2h. The surfaces, with and without biomimetic coating, were characterized by X-ray diffraction analysis and scanning electron microscopy. The relative density was measured by the Archimedes' principle. E and υ were measured by ultrasonic pulse-echo method. For the mechanical properties the specimens (n=30 for each group) were tested in a universal testing machine. RESULTS: Titania addition increased the grain size of the composite and caused a significant decrease in the flexural strength (in MPa, control 815.4a; T10 455.7b and T30 336.0c), E (in GPa, control 213.4a; T10 155.8b and T30 134.0c) and relative density (control 99.0%a; T10 94.4%c and T30 96.3%b) of the Y-TZP/TiO2 composite. The presence of 30% titania caused substantial increase in m and υ. Biomimetic coating did not affect the mechanical properties of the composite. SIGNIFICANCE: The Y-TZP/TiO2 composite coated with a layer of CaP has great potential to be used as implant material. Although addition of titania affected the properties of the composite, the application of a biomimetic coating did not jeopardize its reliability.

Physico-chemical characterization and biocompatibility of hydroxyapatite derived from fish waste.

The aim of this study was to synthesize hydroxyapatite (HAP) powder from fish waste. The powder was characterized through X-ray diffraction, Fourier transform infrared spectroscopy, ion exchange chromatography, scanning electron microscopy and plasma emission spectrometry. The cyto- and genotoxicity was carried out to demonstrate biocompatibility in vivo by means of rat subcutaneous tissue test. The results showed that the visible crystalline nature of typical apatite crystal structure when they were calcined at 800 °C. Infrared spectroscopy analysis showed similar composition to HAP standard with the presence of carbonate ion demonstrated by wave number values of 871 cm-1 and 1420 cm-1 for calcinations at 800 °C. The scanning electronmicrographies depicted the crystal morphology and porous nature with average pore size of ~10 µm. Plasma emission spectrometry and ion exchange chromatography confirmed the presence of Ca and P in the samples. The mean of calcium content was 36.8; Mg was 0.8, Na was 0.7 and K was 0.5. Rat subcutaneous tissue test revealed that HAP presented biocompatibility. Furthermore, the lack of cyto- and genotoxicity in blood, liver, kidney and lung were noticed after 30 days of HAP implantation. Taken together, our results demonstrated that HAP from fish waste exhibits a great potential for using as biomaterial since is represents a simple, effective, low-cost process and satisfactory degree of biocompatibility.