Abstract

The characterisation of cement paste microstructure is an important step towards understanding durability mechanisms in cementitious materials. Scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS) is a widely used technique to analyse the microstructure at the micron-scale. However, it is challenging, notably because the characteristic size of many phases is found on a scale smaller than the EDS interaction volume. This work presents a new image analysis framework to identify phases and quantify the microstructure of cementitious materials from SEM-EDS hypermaps. By leveraging domain knowledge, representative points are attributed to phases and mixtures of phases based on ratio plots. Then, quantitative analysis of the microstructure can be carried out (chemical composition, particle size distributions, volume fractions, …). We demonstrate the abilities of the framework, and we present possible applications and extensions of the method. The framework is available as both a graphical interface and a Python code.

Highlights

  • Scanning electron microscopy (SEM) coupled with electron disper­ sive spectroscopy (EDS) has many applications in cementitious mate­ rials

  • As explained in the previous section, it is possible to identify most of the cement paste phases visible at the backscattered electron (BSE) micrograph scale using a manual selection of points

  • This quantification by image analysis is interesting for several reasons: (1) it provides the apparent volume fraction directly, and not a mass fraction to be transformed into volume fraction; (2) it provides an additional mea­ surement to verify/confirm other methods; and (3) it enables estimation of volume fraction for amorphous phases that cannot be directly measured by X-ray diffraction (XRD)-Rietveld, or by thermogravimetric analyses (TGA) due to peak overlapping

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Summary

Introduction

Scanning electron microscopy (SEM) coupled with electron disper­ sive spectroscopy (EDS) has many applications in cementitious mate­ rials. Cement and Concrete Research 141 (2021) 106327 presented here as a step in the data analysis The importance of these scientific questions over the clustering problem, has led to the combined use of multispectral images (generally qualitative) to study the spatial distribution of phases and, EDS point analyses to study their composi­ tion [5,7,9]. We propose a new approach that allows phase sepa­ ration, chemical analysis, and visualization on the BSE image It ad­ dresses both the physical and the practical challenges of analysing SEMEDS hypermaps of complex cement paste microstructures. Particle shapes and spatial distribution can be analysed from these phase masks This method was implemented into a new framework called edxia, and added into the Glue software [20,21] to make this tool accessible to all researchers. This paper describes the method and some current applications, and aims at setting the stage for further de­ velopments in an open-source framework

Materials
Methods
SEM parameters The majority of SEM-EDS analyses were performed with a Zeiss
Implementation of the edxia method
The edxia method
Denoising of chemical maps
Combination into composite maps
Segmentation of regions with similar compositions
Emulation of point analysis
Characterisation of mixtures
Qualitative phase separation
Chemistry of phases
Sub-resolution phases
Quantitative phase fractions
Microstructure descriptors
Profiles
Using lower-efficiency EDS detectors
Filtering at the spectrum level
Possible extension to machine learning
Concluding remarks
Findings
Code download and installation

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