Characterization of lamellar microstructure of montmorillonite films

doi:10.3785/j.issn.1008-973X.2026.01.020

Journal of ZheJiang University (Engineering Science)

2026, Vol. 60

Issue (1): 208-216 DOI: 10.3785/j.issn.1008-973X.2026.01.020

Characterization of lamellar microstructure of montmorillonite films

Lanyue PENG1,2(

),Yi DONG1,3,*(

)

1. Institute of Rock and Soil Mechanics, Chinese Academy of Sciences, Wuhan 430071, China
2. University of Chinese Academy of Sciences, Beijing 100049, China
3. State Key Laboratory of Geomechanics and Geotechnical Engineering Safety, Wuhan 430071, China

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Abstract

Quantitative analysis was performed on the lamellar thickness and spacing of montmorillonite aggregates in the sodium-based montmorillonite (SWy) and calcium-based montmorillonite (STx) film samples which were prepared via vacuum filtration by combining the scanning electron microscopy (SEM), small-angle X-ray scattering (SAXS) and grazing-incidence small-angle X-ray scattering (GISAXS) techniques and using the methods of SEM image recognition and scattering model fitting, to address the issue that existing characterization techniques struggle to balance the characterization of nanoscale local morphology and the analysis of macroscopic statistical properties. The results demonstrated that the montmorillonite aggregates in SWy films exhibited smaller average lamellar thickness (SEM: 33.73 nm; SAXS: 13.19 nm), with loosely stacked lamellar structures and significant interlayer porosity. The aggregates in STx films formed denser structures due to the ionic bridging effect of Ca²⁺, showing larger lamellar thickness (SEM: 39.23 nm; SAXS: 32.79 nm) and higher dispersion. The combination of SEM-based local morphology analysis, SAXS-based global statistics analysis, and GISAXS-based periodicity analysis enabled the quantitative characterization of feature sizes of the lamellar structures in montmorillonite films and the mutual verification of data reliability. The analysis results demonstrated the feasibility of this combined method in providing technical support for the directional design of functional montmorillonite films by integrating multi-scale structural information.

Key words： montmorillonite film lamellar structure microstructural characterization small angle X-ray scattering grazing-incidence small-angle X-ray scattering

Received: 15 March 2024 Published: 15 December 2025

CLC:

TB 303

Fund: 国家自然科学基金资助项目（42277178, 51779254）.

Corresponding Authors: Yi DONG E-mail: penglanyue22@mails.ucas.ac.cn;ydong@whrsm.ac.cn

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Cite this article:

Lanyue PENG,Yi DONG. Characterization of lamellar microstructure of montmorillonite films. Journal of ZheJiang University (Engineering Science), 2026, 60(1): 208-216.

URL:

https://www.zjujournals.com/eng/10.3785/j.issn.1008-973X.2026.01.020 OR https://www.zjujournals.com/eng/Y2026/V60/I1/208

蒙脱土薄膜层状微观结构表征

针对现有表征技术难以兼顾纳米级局部形貌表征与宏观统计特性分析的问题，采用真空抽滤法制备钠基蒙脱土（SWy）与钙基蒙脱土（STx）薄膜样品，通过联用扫描电镜（SEM）、小角X射线散射（SAXS）和掠入式小角X射线散射（GISAXS）技术，运用SEM图像识别与散射模型拟合方法，对蒙脱土类聚体的层厚和间距开展定量解析. 结果表明，SWy薄膜类聚体的平均层厚更小（SEM: 33.73 nm; SAXS: 13.19 nm），呈松散层状堆叠，层间孔隙显著. STx薄膜中的类聚体因Ca²⁺的离子桥联效应形成更致密的结构，平均层厚更大（SEM: 39.23 nm; SAXS: 32.79 nm），离散性更高. SEM局部形貌分析、SAXS全局统计分析及GISAXS周期性分析的联用实现了蒙脱土薄膜层状结构特征尺寸的定量表征，且能够互相验证数据的可靠性. 分析结果验证了该联用方法通过融合多尺度结构信息为蒙脱土功能薄膜定向设计提供技术支撑的可行性.

关键词： 蒙脱土薄膜, 层状结构, 微观结构表征, 小角X射线散射, 掠入式小角X射线散射

Fig.1 Preparation process of layered clay film

Fig.2 Schematic diagram of SAXS/GISAXS

Fig.3 TEM analysis results of montmorillonite aggregates

Fig.4 Photographs of montmorillonite films

Fig.5 SEM images of lamellar microstructure of montmorillonite films

Fig.6 Image recognition and processing process for lamellar thickness acquisition based on SEM results

Fig.7 Characterization of lamellar thickness distribution of montmorillonite films based on SEM image recognition

Tab.1 SEM/SAXS/GISAXS-based feature sizes and related parameters of sodium-based and calcium-based montmorillonite

Fig.8 SAXS 2D patterns, 1D intensity curves and model fitting curves

Fig.9 Lamellar thickness distribution obtained by model fitting of SAXS intensity curves

Fig.10 PDDF curves of montmorillonite films

Fig.11 GISAXS 2D patterns and 1D intensity curves of montmorillonite films


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