New solvothermal flow synthesis of strontium titanate nanoparticles based on the use of acetylacetonate precursors in water/ethanol mixture

IF 3.4 3区 工程技术 Q2 CHEMISTRY, PHYSICAL Journal of Supercritical Fluids Pub Date : 2024-07-14 DOI:10.1016/j.supflu.2024.106353
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Abstract

In this study, strontium titanate (SrTiO3) nanoparticles were obtained utilizing a one-step supercritical continuous solvothermal synthesis process involving acetylacetonate precursors for both strontium and titanium cations instead of the historical alkoxide ones. These precursors are expensive, difficult to access (especially for strontium isopropoxyde) and inadequately stable, forcing the use of a glove box and controlled atmospheres, which is not the case for acetylacetonates. Pure SrTiO3 nanoparticles with a crystallite size of roughly 20 nm were successfully synthesized. In addition to the cubic structure of SrTiO3, FTIR revealed surface functions that are typical of "wet" processes, while Raman spectroscopy showed the activation of non-centrosymmetric modes brought on by non-linear contributions. The nanoparticles show a faceted shape and are stable at elevated temperatures (up to 800 °C), according to in-situ high temperature XRD measurements. However, due to a chemical deficiency in strontium, titanium dioxide (TiO2) phases are formed at higher temperatures. In-situ high temperature HRTEM investigations showed the existence of two populations of particles, with a better stability for the bigger-sized particles after thermal treatment as well as the sintering and restructuring of the smallest ones. Also, the microscopy results suggest the possibility of a chemical inhomogeneity within the crystallites. Overall, this study offers important new knowledge on the physicochemical characteristics of the synthesized SrTiO3 nanoparticles and their thermal stability using a novel supercritical continuous solvothermal approach based on the use of acetylacetonate precursors.

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基于在水/乙醇混合物中使用乙酰丙酮前体的新型溶热流法合成纳米钛酸锶颗粒
本研究采用一步超临界连续溶热合成工艺获得了钛酸锶(SrTiO3)纳米粒子,该工艺使用乙酰丙酮酸盐作为锶和钛阳离子的前驱体,而不是传统的氧化烷。这些前驱体价格昂贵、难以获得(尤其是异丙醇锶)且不够稳定,因此必须使用手套箱和可控气氛,而乙酰丙酮则不然。我们成功合成了结晶尺寸约为 20 纳米的纯 SrTiO3 纳米粒子。除了 SrTiO3 的立方结构外,傅立叶变换红外光谱还显示了典型的 "湿 "过程表面功能,而拉曼光谱则显示了非线性贡献带来的非中心对称模式的激活。根据原位高温 XRD 测量,纳米颗粒呈现出刻面形状,并在高温(高达 800 ℃)下保持稳定。然而,由于锶的化学性质不足,在较高温度下会形成二氧化钛(TiO2)相。原位高温 HRTEM 研究表明,存在两种颗粒群,尺寸较大的颗粒在热处理后具有更好的稳定性,而尺寸较小的颗粒则会烧结和重组。此外,显微镜观察结果表明晶体内部可能存在化学不均匀性。总之,这项研究提供了重要的新知识,即使用基于乙酰丙酮前驱体的新型超临界连续溶热方法合成的 SrTiO3 纳米粒子的物理化学特性及其热稳定性。
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来源期刊
Journal of Supercritical Fluids
Journal of Supercritical Fluids 工程技术-工程:化工
CiteScore
7.60
自引率
10.30%
发文量
236
审稿时长
56 days
期刊介绍: The Journal of Supercritical Fluids is an international journal devoted to the fundamental and applied aspects of supercritical fluids and processes. Its aim is to provide a focused platform for academic and industrial researchers to report their findings and to have ready access to the advances in this rapidly growing field. Its coverage is multidisciplinary and includes both basic and applied topics. Thermodynamics and phase equilibria, reaction kinetics and rate processes, thermal and transport properties, and all topics related to processing such as separations (extraction, fractionation, purification, chromatography) nucleation and impregnation are within the scope. Accounts of specific engineering applications such as those encountered in food, fuel, natural products, minerals, pharmaceuticals and polymer industries are included. Topics related to high pressure equipment design, analytical techniques, sensors, and process control methodologies are also within the scope of the journal.
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