Live SEM EDS Enhances the Microstructure Analysis of Steel

Microstructural analysis of advanced materials

There is a rising demand for advanced materials as industries increasingly require ever more tightly controlled and reliable physical properties to produce next-generation components, devices, and products. For instance, there has been a push for higher performance and durability in aerospace structures, as well as a need for lighter and stronger materials in electric vehicles, along with general improvements in energy efficiency and sustainability across industries, particularly in consumer electronics. Additionally, lightweight composites and high-performance alloys have proven to be essential for reducing fuel consumption and enhancing safety in aircraft and defense platforms. The bulk characteristics of these materials are ultimately a consequence of microscopic variations in their composition, and as a result, microstructural analysis is becoming a growing necessity across materials manufacturing and research.

This is particularly true in metallurgy, where particles and inclusions in the bulk metal have profound impacts on the material’s overall behavior. Imaging, even at high resolutions, can often only tell part of the story, even with techniques such as backscattered electron imaging in scanning electron microscopy (SEM), in which image grayscale is reflective of compositional contrast. Inclusions may blend into the background if they are close in atomic number to the bulk metal, whereas particles consisting of elements with similar atomic numbers may be indistinguishable. This is why truly robust characterization combines information from multiple complementary analytical techniques. For instance, energy-dispersive X-ray spectroscopy (EDS) can be performed within the same electron microscope as SEM, and provides chemical identification of the sample surface.

SEM EDS microstructure analysis of a steel inclusion obtained with the Axia ChemiSEM.
Steel inclusion analysis with live, simultaneous SEM imaging and EDS elemental analysis. The EDS spectrum confirms the presence of bulk iron as well as chromium, carbon, silicon, manganese, sulfur, and nickel.

Scanning electron microscopy and energy-dispersive X-ray spectroscopy

Historically, the combination of SEM and EDS data required two separate acquisition sessions, resulting in a lengthy and complex analytical workflow. Advances in both hardware and software allowed this data to be acquired simultaneously using a system of detectors, but even this had to be followed by an extended post-processing step where the EDS data is aligned with the SEM image. Today, further refinement of these workflows, along with AI-powered automation, has resulted in truly “real-time” correlation and visualization of SEM-EDS data. This is showcased in specialized instrumentation such as the Thermo Scientific™ Axia™ ChemiSEM System, which combines imaging and elemental analysis into a single, automated workflow.

Microstructural analysis of steel inclusions

The Axia ChemiSEM System is a versatile tool capable of microstructural analysis across a range of samples, from polymers to ceramics, metals, and soft materials, as well as micro- and nano-particles, and more. Here, inclusions in a steel sample will be highlighted, as steel is one of the most widely used metals across multiple industries, including aerospace and automotive manufacturing, oil and gas, etc. Inclusions play a critical role in the mechanical properties and durability of steel, so their accurate characterization is critical for evaluating and optimizing the metal.

To enable the examination of a wide variety of materials and applications, the Axia ChemiSEM System features a large sample chamber capable of supporting up to 10 kg. It can fit 7 mounted SEM stubs, and larger samples (such as the 5×5 cm stainless steel sample investigated here) can be mounted directly onto the stage. It can also support a variety of sample holders (such as multi-stub holders) that accommodate a range of common specimen types, including resin-mounted samples. As these holders contain multiple samples at a time, this facilitates routine analysis, which is particularly useful for particle characterization in QA, QC, and failure analysis.

Once the sample is loaded, the user only needs to click on an area of interest in the navigation camera image (which serves as a map overview) to drive to that specific location and immediately begin acquiring simultaneous SEM and EDS data. This live multimodal analysis helps ensure inclusions are classified based on both morphology and chemistry, which is critical for reproducible quality control and standards-based reporting.

SEM-EDS data analyzed further in the offline ChemiViewer of the ChemiSEM System. Corroborating the observations made during data collection, greater concentrations of manganese and sulfur are seen within the inclusion compared to the bulk, strongly suggesting that this is a manganese sulfide inclusion. Line scans can also be performed to show how elemental concentrations change across the image. A line across the manganese sulfide particle shows the concentration of iron decreases as the concentrations of manganese and sulfur increase.

Perspectives on live SEM-EDS for microstructural analysis

Live, automated SEM-EDS workflows, as enabled by the Axia ChemiSEM System, allow engineers and QA teams to move beyond selective inspection toward comprehensive, large-area analysis with consistent detection and classification. The Axia ChemiSEM System inherently captures and correlates elemental and structural information throughout the imaging process, revealing vital microstructural variability and details such as particle and inclusion composition. This provides actionable metrics that support decision-making across the value chain, from R&D to failure analysis and process optimization. As microstructural analysis becomes increasingly critical, the availability of tools that simplify and automate this characterization will be ever more vital for materials manufacturers and researchers. SEM-EDS analysis with the Axia ChemiSEM System facilitates exactly such workflows through its unique combination of advanced hardware and automation software.

Watch our on-demand webinar to learn more about microstructural analysis with the Axia ChemiSEM System >

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