Facile synthesis and characterization of ZrO₂nanoparticles prepared by the AOP/hydrothermal route

Abstract

We report on the synthesis and characterization of ZrO 2 nanoparticles prepared from zirconium(IV) butoxide in the absence of base or acid mineraliser by an advanced oxidation processes (AOP) and subsequent hydrothermal treatment which involves mixing and dissolution of the precursor for different temperatures. The structure, morphology and properties of the nanoparticles were characterized using XRD, FE-SEM, TEM, HRTEM, Raman spectroscopy, FT-IR spectroscopy, BET measurements and TGA measurements. The structural analysis by XRD and Raman spectroscopy confirms the ZrO 2 specimens synthesized at 100 C for 1 hour are amorphous and those treated at 150 C and 200 C for 1 hour were crystalline. Structural analysis by Raman spectroscopy confirms tetragonal ZrO 2 specimens obtained at temperatures higher than 100 C as a majority phase. From FE-SEM images, the AOP/hydrothermal route mainly produced microspheres comprised of primary nanoparticles. HRTEM images of ZrO 2 microspheres, after treatment at 100 C, show the beginning of crystallization, with only a few clear lattice fringes dispersed in the specimens. TEM and HRTEM images of ZrO 2 , after treatment at 150 C and 200 C indicate that the microspheres are the aggregation of small nanoparticles with a size of approximately 5-8 nm, and FFT analysis confirms the high crystallinity of the specimens. TGA analyses show a distinctive behavior for each of the ZrO 2 specimens, after treatment at 100 C, 150 C and 200 C. FT-IR analysis of ZrO 2 specimens after hydrothermal treatment revealed the presence of groups, such as -OH, -CH 2 , and -CH at the surface. In addition, FT-IR spectra show a decrease in the amount of functional groups attached to the surface of the nanoparticles when the reaction temperature is increased. This result was also confirmed by TGA analysis. The ZrO 2 specimens prepared by the AOP/ hydrothermal route exhibited a high surface area of 511-184 m 2 g À1 .

Interaction between Amorphous Zirconia Nanoparticles and Graphite: Electrochemical Applications for Gallic Acid Sensing Using Carbon Paste Electrodes in Wine

“…The ZrO 2 nanoparticles modified CPE was characterised by first studying the sizes of the ZrO 2 nanoparticles using a Zetasizer. The sizes were recorded and ranged between 20 to 470 nm, which is in line with other works in the literature, where their synthesis produced sizes ranging from 10 to 400 nm [39,40].…”

“…in line with other works in the literature, where their synthesis produced sizes ranging from 10 to 400 nm [39,40]. SEM provides information on the external morphology, chemical composition, and crystalline structure of the ZrO2 nanoparticles.…”

The Effect of Addition of Nanoparticles, Especially ZrO2-Based, on Tribological Behavior of Lubricants

“…Padovini et al [54] analyzed a hydrothermal zirconia nanoparticle synthesis and found that ZrO 2 nanoparticles directly formed amorphous microspheres before the primary particles crystallized within these structures.…”

Fractal growth of ZrO2nanoparticles induced by synthesis conditions

“…Furthermore, the values are also in good agreement with other specific surface area values reported for ZrO 2 nanoparticles in the literature. 53,54 Verma et al synthesized ZrO 2 nanoparticles using a reactive magnetron sputtering technique and were able to adjust the specific surface area from 119.81 to 48.89 m 2 g −1 by a subsequent annealing treatment at different temperatures. Here, adjusting the specific surface area of the nanoparticles can be achieved directly through controlling the growth conditions by temperature.…”