A Versatile MEMS-Based In Situ SEM Holder for Heating, Biasing, and Correlative Microstructural Characterization

Microscopy and Microanalysis, vol. 31

Abstract

In situ scanning electron microscopy (SEM) is increasingly attracting interest, as it provides invaluable insights into the real-time evolution of materials under external stimuli like heating, electrical biasing, and mechanical stress. Such dynamic experiments bridge the gap between ex situ characterization and real-world applications for topics like pyrolysis [1], the microstructural evolution in steels during heat treatment [2], electrothermal responses of metals and semiconductors [2], additive manufacturing [3], and morphological studies of catalysts [4], among others. Additionally, in situ SEM serves as a powerful complementary technique to transmission electron microscopy (TEM). It enables studying microstructural changes and surface dynamics observed at lower magnifications in SEM, before being further examined in greater detail using TEM, thus providing multiscale insights into materials. This work presents a MEMS-based holder compatible with SEM and Dual Beam systems enabling in situ heating, biasing, and microstructural characterization. This development aims to capitalize on the flexible work environment and variety of detectors available for SEMs, thus enabling correlative in situ studies using techniques, including energy-dispersive X-ray spectroscopy (EDX), electron backscatter diffraction (EBSD), and transmission Kikuchi diffraction (TKD) [2], offering elemental and crystallographic information, to further enhance our understanding of material responses to thermal and electrical conditions. This multi-technique compatibility is ensured by designing the SEM holder to employ the same heating and/or biasing MEMS Nano-Chips used by in situ TEM holders in a way that seamlessly allows beam transmission, facilitating cross-platform and multiscale correlative analysis. Additionally, this study aims to evaluate the SEM holder in combination with correlative atomic force microscopy (AFM) integrated into SEM stages. To demonstrate the performance and flexibility of the in situ SEM stage, the in situ heating and biasing holder for SEM was utilized to investigate the thermal and electrical response of various samples, prepared onto Heating and/or Biasing Nano-Chips. Microstructural characterization, combined with in situ heating was performed using both on-axis and off-axis EBSD detectors. A number of SEM/Dual Beam systems from different brands were employed in conjunction with an AFM stage for performing these in situ and correlative experiments. This versatile SEM stage enables real-time analysis of phase transformations, grain evolution, and defect dynamics under controlled thermal and electrical conditions, and grain evolution using EBSD and TKD, allowing for operando studies of material behavior at the microscale. Furthermore, it facilitates correlative microscopy studies by integrating SEM and AFM signals, while also allowing seamless sample transfer to TEM without compromising microstructural integrity. Case studies on various materials demonstrate the system’s ability to capture fine-scale structural changes with high spatial and temporal resolution. Its cross-platform compatibility and correlative characterization capabilities bridge the gap between SEM, AFM, and TEM studies. This work paves the way for future research integrating multimodal in situ techniques, providing a more comprehensive understanding of dynamic material processes.

Authors 7

1. Yevheniy V. Pivak

   Denssolutions (Netherlands)

   Affiliation as printed

   DENSsolutions B.V., Informaticalaan 12 , 2628 ZD Delft ,

2. Christian Deen-van-Rossum

   Denssolutions (Netherlands)

   Affiliation as printed

   DENSsolutions B.V., Informaticalaan 12 , 2628 ZD Delft ,

3. Mia Andersen

   Denssolutions (Netherlands)

   Affiliation as printed

   DENSsolutions B.V., Informaticalaan 12 , 2628 ZD Delft ,

4. Merijn Pen

   Denssolutions (Netherlands)

   Affiliation as printed

   DENSsolutions B.V., Informaticalaan 12 , 2628 ZD Delft ,

5. Shibabrata Basak

   Forschungszentrum Jülich

   Affiliation as printed

   Institute of Energy Technologies - Fundamental Electrochemistry (IET-1) , Forschungszentrum Jülich GmbH, Jülich ,

6. Rüdiger‐A. Eichel Aachen Faculty of Mechanical Engineering Institute of Physical Chemistry

   RWTH Aachen University · Forschungszentrum Jülich

   Affiliation as printed

   Faculty of Mechanical Engineering, RWTH Aachen University , Aachen ,

   Institute of Energy Technologies - Fundamental Electrochemistry (IET-1) , Forschungszentrum Jülich GmbH, Jülich ,

   Institute of Physical Chemistry, RWTH Aachen University , Aachen ,

7. H. Hugo Pérez Garza

   Denssolutions (Netherlands)

   Affiliation as printed

   DENSsolutions B.V., Informaticalaan 12 , 2628 ZD Delft ,