de Vos Wiebe M, Mears Laura L E, Richardson Robert M, Cosgrove Terence, Dalgliesh Robert M, Prescott Stuart W
School of Chemistry, University of Bristol, Cantock's close, BS8 1TS Bristol, United Kingdom.
Rev Sci Instrum. 2012 Nov;83(11):113903. doi: 10.1063/1.4767238.
A unique surface force type apparatus that allows the investigation of a confined thin film using neutron reflection is described. The central feature of the setup consists of a solid substrate (silicon) and a flexible polymer membrane (Melinex(®)). We show that inflation of the membrane against the solid surface provides close and even contact between the interfaces over a large surface area. Both heavy water and air can be completely squeezed out from between the flexible film and the solid substrate, leaving them in molecular contact. The strength of confinement is controlled by the pressure used to inflate the membrane. Dust provides a small problem for this approach as it can get trapped between membrane and substrate to prevent a small part of the membrane from making good contact with the substrate. This results in the measured neutron reflectivity containing a small component of an unwanted reflection, between 10% and 20% at low confining pressures (1 bar) and between 1% and 5% at high confining pressures (5 bar). However, we show that this extra signal does not prevent good and clear information on the structure of thin films being extracted from the neutron reflectivity. The effects of confinement are illustrated with data from a poly(vinyl pyrollidone) gel layer in water, a polyelectrolyte multilayer in water, and with data from a stack of supported lipid-bilayers swollen with D(2)O vapor. The data demonstrates the potential of this apparatus to provide information on the structure of thin films under confinement for a known confining pressure.
本文描述了一种独特的表面力型仪器,该仪器可利用中子反射研究受限薄膜。该装置的核心部件包括一个固体基板(硅)和一个柔性聚合物膜(麦拉宁(®))。我们发现,将膜压向固体表面会使界面在大面积上紧密且均匀地接触。重水和空气都能从柔性膜与固体基板之间被完全挤出,使它们处于分子接触状态。限制强度由用于给膜充气的压力控制。灰尘给这种方法带来了一个小问题,因为它可能被困在膜和基板之间,导致膜的一小部分无法与基板良好接触。这使得测得的中子反射率包含一小部分不需要的反射,在低限制压力(1巴)下为10%至20%,在高限制压力(5巴)下为1%至5%。然而,我们表明,这种额外的信号并不妨碍从中子反射率中提取关于薄膜结构的清晰有效信息。通过水中的聚乙烯吡咯烷酮凝胶层、水中的聚电解质多层膜的数据,以及用D(2)O蒸汽溶胀的支撑脂质双层堆栈的数据,说明了限制效应。这些数据证明了该仪器在已知限制压力下提供关于受限薄膜结构信息的潜力。