{"title":"New solvothermal flow synthesis of strontium titanate nanoparticles based on the use of acetylacetonate precursors in water/ethanol mixture","authors":"","doi":"10.1016/j.supflu.2024.106353","DOIUrl":null,"url":null,"abstract":"<div><p>In this study, strontium titanate (SrTiO<sub>3</sub>) 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 SrTiO<sub>3</sub> nanoparticles with a crystallite size of roughly 20 nm were successfully synthesized. In addition to the cubic structure of SrTiO<sub>3</sub>, 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 <em>in-situ</em> high temperature XRD measurements. However, due to a chemical deficiency in strontium, titanium dioxide (TiO<sub>2</sub>) phases are formed at higher temperatures. <em>In-situ</em> 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 SrTiO<sub>3</sub> nanoparticles and their thermal stability using a novel supercritical continuous solvothermal approach based on the use of acetylacetonate precursors.</p></div>","PeriodicalId":17078,"journal":{"name":"Journal of Supercritical Fluids","volume":null,"pages":null},"PeriodicalIF":3.4000,"publicationDate":"2024-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S0896844624001888/pdfft?md5=3dcb0274f24be3641efa8c8216d528e2&pid=1-s2.0-S0896844624001888-main.pdf","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Supercritical Fluids","FirstCategoryId":"5","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0896844624001888","RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, PHYSICAL","Score":null,"Total":0}
引用次数: 0
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.
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.