Toth Kristof, Osuji Chinedum O, Yager Kevin G, Doerk Gregory S
Department of Chemical and Environmental Engineering, Yale University, New Haven, Connecticut 06520, USA.
Department of Chemical and Biomolecular Engineering, University of Pennsylvania, Philadelphia, Pennsylvania 19104, USA.
Rev Sci Instrum. 2020 Jan 1;91(1):013701. doi: 10.1063/1.5129625.
Electrospray deposition (ESD) enables the growth of solution deposited thin films in a precise and continuous manner by the delivery of submicron droplets of dilute solutions to a heated substrate. By combining ESD with programmable motor control and gradient solution pumping in a first-of-its-kind user tool at the Center for Functional Nanomaterials at Brookhaven National Laboratory, we show the ability to create one or two dimensional compositional gradient nanoscale films via ESD. These capabilities make it possible to construct thin film multicomponent "libraries" on a single substrate to rapidly and systematically characterize composition-dependent properties in a variety of material systems such as thin films involving homopolymer and block copolymer blends. We report the design, construction, and validation of a gradient ESD tool that allows users to carefully control the jet stability, flow composition, spray position, and substrate temperature. Calibrated thin films range in thickness from tens to hundreds of nanometers. We demonstrate gradient thin films using a ternary dye triangle as well as a gradual blending of polystyrene homopolymer with poly(styrene-block-methyl methacrylate) on a single substrate. Paired with the rapid measurement capabilities of synchrotron small angle X-ray scattering, this tool forms an integral part of a new platform for high-throughput, autonomous characterization and design of nanomaterial thin films and soft materials more generally.
电喷雾沉积(ESD)通过将稀溶液的亚微米液滴输送到加热的基板上,能够以精确且连续的方式生长溶液沉积薄膜。通过在布鲁克海文国家实验室功能纳米材料中心的一款首创的用户工具中,将ESD与可编程电机控制和梯度溶液泵送相结合,我们展示了通过ESD创建一维或二维成分梯度纳米级薄膜的能力。这些能力使得在单个基板上构建薄膜多组分“库”成为可能,从而能够快速且系统地表征各种材料体系中与成分相关的特性,例如涉及均聚物和嵌段共聚物共混物的薄膜。我们报告了一种梯度ESD工具的设计、构建和验证,该工具允许用户仔细控制喷射稳定性、流动成分、喷雾位置和基板温度。校准后的薄膜厚度范围从几十纳米到几百纳米。我们展示了使用三元染料三角形以及在单个基板上聚苯乙烯均聚物与聚(苯乙烯 - 嵌段 - 甲基丙烯酸甲酯)的逐渐共混制备的梯度薄膜。与同步加速器小角X射线散射的快速测量能力相结合,该工具构成了一个新平台的重要组成部分,该平台可更广泛地用于纳米材料薄膜和软材料的高通量、自主表征与设计。