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Synthesis of Elusive Monoclinic ZrO2 Nanostructures via Hydrothermal Treatment
Journal of Inorganic and Organometallic Polymers and Materials ( IF 3.9 ) Pub Date : 2023-05-14 , DOI: 10.1007/s10904-023-02686-w
Sakshi Thakur , Shweta Sareen , Meenakshi Verma , Kirtanjot Kaur , Vishal Mutreja

ZrO2 is considered an important semiconductor and a heterogeneous photocatalyst along with its diversified applications in dentistry and ceramics. In the present study, ZrO2 nanostructures were synthesized by hydrothermal treatment accompanied by calcination at different temperatures, viz. 300–800 °C, using zirconyl chloride octahydrate as a precursor, and pure phytochemical- catechin hydrate as a stabilizing agent. Significant variations in the optical properties viz. absorption spectra, and band gap; and structural properties viz. average particle, and crystallite size of ZrO2 nanostructures were observed due to variable calcination temperatures. The diffraction studies showed that crystallinity appeared in samples synthesized at or above 400 °C. The lowest average crystallite sizes of ~8.96 nm and ~14.5 nm were obtained for the ZrO2 synthesized at calcination temperatures of 400 and 500 °C, respectively. The obtained XRD data of ZrO2 nanostructures were further studied by Rietveld refinement using various space groups viz., Fm-3 m for cubic, P121/c1 for monoclinic, and P42/nmc for tetragonal phases. The refinement illustrated the development of the monoclinic phase of ZrO2 in major composition, for the samples synthesized at or above 400 °C, with preferred orientations along (011), (111), and (1̅11). Furthermore, the HRTEM data showed the formation of the spherical particles with average particle sizes of ~ 47 nm and ~26 nm, prepared at 500 and 600 °C, respectively. Theoretical studies were also carried out to get a mechanistic understanding of the procedure followed in the synthesis and stability of the zirconia nanoparticles. The prepared ZrO2 nanostructures were further investigated for their photodegradable capability of tetracycline hydrochloride (TCH) under visible light irradiation. Among all the prepared materials, ZrO2 prepared at 500 °C exhibited a higher photo-degradation efficiency at 180 min under visible light irradiation.

Graphical Abstract



中文翻译:

通过水热处理合成难以捉摸的单斜 ZrO2 纳米结构

ZrO 2被认为是一种重要的半导体和多相光催化剂,以及它在牙科和陶瓷领域的多样化应用。在本研究中,ZrO 2纳米结构是通过水热处理伴随不同温度下的煅烧合成的,即。300–800 °C,以八水氯氧锆为前体,纯植物化学-儿茶素水合物为稳定剂。光学特性的显着变化即。吸收光谱和带隙;和结构特性即 ZrO 2的平均粒径和微晶尺寸由于不同的煅烧温度,观察到纳米结构。衍射研究表明,在 400 °C 或以上合成的样品中出现结晶。在 400 和 500 °C 的煅烧温度下合成的 ZrO 2分别获得了~8.96 nm 和~14.5 nm 的最低平均微晶尺寸。获得的 ZrO 2纳米结构的 XRD 数据通过 Rietveld 精修使用各种空间群进一步研究,即立方相的 Fm-3 m、单斜相的 P121/c1 和四方相的 P42/nmc。细化说明了 ZrO 2的单斜晶相的发展在主要成分中,对于在 400 °C 或更高温度下合成的样品,具有沿 (011)、(111) 和 (1̅11) 的优选方向。此外,HRTEM 数据显示分别在 500 和 600 °C 下制备的平均粒径为 ~ 47 nm 和 ~ 26 nm 的球形颗粒的形成。还进行了理论研究,以获得对氧化锆纳米粒子的合成和稳定性所遵循的程序的机械理解。进一步研究制备的 ZrO 2纳米结构在可见光照射下对四环素盐酸盐 (TCH) 的光降解能力。在所有制备的材料中,在 500 °C 下制备的 ZrO 2在可见光照射下 180 分钟时表现出更高的光降解效率。

图形概要

更新日期:2023-05-15
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