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浙江大学学报(工学版)
浙江大学学报(工学版)  2026, Vol. 60 Issue (1): 208-216    DOI: 10.3785/j.issn.1008-973X.2026.01.020
土木工程     
蒙脱土薄膜层状微观结构表征
彭兰月1,2(),董毅1,3,*()
1. 中国科学院武汉岩土力学研究所，湖北 武汉 430071
2. 中国科学院大学，北京 100049
3. 岩土力学与工程安全全国重点实验室，湖北 武汉 430071
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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摘要：

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    
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
收稿日期: 2024-03-15 出版日期: 2025-12-15
:  TB 303  
基金资助: 国家自然科学基金资助项目（42277178, 51779254）.
通讯作者: 董毅     E-mail: penglanyue22@mails.ucas.ac.cn;ydong@whrsm.ac.cn
作者简介: 彭兰月（2000—），女，硕士生，从事非饱和土吸附行为研究. orcid.org/0009-0002-6762-2624. E-mail：penglanyue22@mails.ucas.ac.cn
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引用本文:

彭兰月,董毅. 蒙脱土薄膜层状微观结构表征[J]. 浙江大学学报(工学版), 2026, 60(1): 208-216.

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

链接本文:

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

图 1  层状黏土薄膜制备流程
图 2  小角X射线散射/掠入式小角X射线散射原理图
图 3  蒙脱土类聚体的透射电子显微镜分析结果
图 4  蒙脱土薄膜实物照片
图 5  蒙脱土薄膜层状微观结构的扫描电镜图像
图 6  基于SEM结果获得层厚的图像识别与处理流程
图 7  基于SEM图像识别的蒙脱土薄膜片层厚度分布表征
样品SEM图像识别SEM LogNormal拟合SAXS模型拟合SAXS PDDFGISAXS
tm/nmμσμσR/nmtm/nmds/nmdB/nm
SWy33.7331.640.1612.180.40431.9313.1920.0225.86
STx39.2336.600.2128.030.56634.9032.7924.0136.11
表 1  基于SEM/SAXS/GISAXS的钠基和钙基蒙脱土特征尺寸和相关参数
图 8  SAXS二维图谱、一维强度曲线和模型拟合曲线
图 9  SAXS强度曲线经模型拟合所得的片层厚度分布
图 10  蒙脱土薄膜的对距离分布函数曲线
图 11  蒙脱土薄膜的GISAXS二维图谱及一维散射强度曲线
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