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一种通过小角中子散射研究纳米多孔氧化铝的新方法。

A novel methodology to study nanoporous alumina by small-angle neutron scattering.

作者信息

Christoulaki Anastasia, Chennevière Alexis, Grillo Isabelle, Porcar Lionel, Dubois Emmanuelle, Jouault Nicolas

机构信息

Sorbonne Université, CNRS, Laboratoire Physicochimie des Electrolytes et des Nanosystèmes Interfaciaux, PHENIX, F-75005 Paris, France.

Laboratoire Léon Brillouin (LLB), CEA Saclay, 91191 Gif-Sur-Yvette, France.

出版信息

J Appl Crystallogr. 2019 Jun 28;52(Pt 4):745-754. doi: 10.1107/S160057671900726X. eCollection 2019 Aug 1.

Abstract

Nanoporous anodic aluminium oxide (AAO) membranes are promising host systems for confinement of condensed matter. Characterizing their structure and composition is thus of primary importance for studying the behavior of confined objects. Here a novel methodology to extract quantitative information on the structure and composition of well defined AAO membranes by combining small-angle neutron scattering (SANS) measurements and scanning electron microscopy (SEM) imaging is reported. In particular, (i) information about the pore hexagonal arrangement is extracted from SEM analysis, (ii) the best SANS experimental conditions to perform reliable measurements are determined and (iii) a detailed fitting method is proposed, in which the probed length in the fitting model is a critical parameter related to the longitudinal pore ordering. Finally, to validate this strategy, it is applied to characterize AAOs prepared under different conditions and it is shown that the experimental SANS data can be fully reproduced by a core/shell model, indicating the existence of a contaminated shell. This original approach, based on a detailed and complete description of the SANS data, can be applied to a variety of confining media and will allow the further investigation of condensed matter under confinement.

摘要

纳米多孔阳极氧化铝(AAO)膜是用于限制凝聚态物质的有前景的主体体系。因此,表征其结构和组成对于研究受限物体的行为至关重要。本文报道了一种通过结合小角中子散射(SANS)测量和扫描电子显微镜(SEM)成像来提取关于明确AAO膜结构和组成的定量信息的新方法。具体而言,(i)从SEM分析中提取有关孔六边形排列的信息,(ii)确定进行可靠测量的最佳SANS实验条件,以及(iii)提出一种详细的拟合方法,其中拟合模型中的探测长度是与纵向孔有序相关的关键参数。最后,为验证该策略,将其应用于表征在不同条件下制备的AAO,结果表明实验SANS数据可以由核/壳模型完全重现,表明存在受污染的壳层。这种基于对SANS数据详细完整描述的原始方法可应用于各种限制介质,并将有助于进一步研究受限条件下的凝聚态物质。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f2a7/6662990/c2464bd03757/j-52-00745-fig1.jpg

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