Barker Connor R, Lewns Francesca K, Poologasundarampillai Gowsihan, Ward Andrew D
Department of Earth Sciences, Royal Holloway University of London, Queens Building, Egham, Surrey TW20 0EX, U.K.
STFC, Central Laser Facility, Research Complex at Harwell, Rutherford Appleton Laboratory, Didcot, Oxfordshire, OX11 0FA, U.K.
ACS Appl Nano Mater. 2022 Aug 26;5(8):11699-11706. doi: 10.1021/acsanm.2c02683. Epub 2022 Aug 17.
Optical trapping enables the real-time manipulation and observation of morphological evolution of individual particles during reaction chemistry. Here, optical trapping was used in combination with Raman spectroscopy to conduct airborne assembly and kinetic experiments. Micro-droplets of alkoxysilane were levitated in air prior to undergoing either acid- or base-catalyzed sol-gel reaction chemistry to form silica particles. The evolution of the reaction was monitored in real-time; Raman and Mie spectroscopies confirmed the in situ formation of silica particles from alkoxysilane droplets as the product of successive hydrolysis and condensation reactions, with faster reaction kinetics in acid catalysis. Hydrolysis and condensation were accompanied by a reduction in droplet volume and silica formation. Two airborne particles undergoing solidification could be assembled into unique 3D structures such as dumb-bell shapes by manipulating a controlled collision. Our results provide a pipeline combining spectroscopy with optical microscopy and nanoscale FIB-SEM imaging to enable chemical and structural insights, with the opportunity to apply this methodology to probe structure formation during reactive inkjet printing.
光镊技术能够在反应化学过程中对单个粒子的形态演变进行实时操控和观察。在此,光镊技术与拉曼光谱联用,用于进行气载组装和动力学实验。在进行酸催化或碱催化的溶胶 - 凝胶反应化学以形成二氧化硅颗粒之前,烷氧基硅烷的微滴悬浮于空气中。反应过程实时监测;拉曼光谱和米氏光谱证实,烷氧基硅烷液滴通过连续的水解和缩合反应原位形成二氧化硅颗粒,酸催化下反应动力学更快。水解和缩合伴随着液滴体积减小和二氧化硅形成。通过控制碰撞操作,两个正在固化的气载颗粒可组装成独特的三维结构,如哑铃形状。我们的结果提供了一种将光谱学与光学显微镜以及纳米级聚焦离子束扫描电子显微镜成像相结合的方法,以实现化学和结构方面的深入了解,并有机会将该方法应用于探测反应性喷墨打印过程中的结构形成。