Automated SEM and nanoindentation at NIMS Japan: Accelerating alloy discovery

What if you could condense years of materials testing into just 13 days? At the National Institute for Materials Science (NIMS) in Japan, researchers have done exactly that. By transforming a process that traditionally takes over seven years into an automated workflow, they are reshaping the development of aerospace materials.

At NIMS’s Research Center for Structural Materials (RCSM), a team led by Toshio Osada in the High-Reliability Heat-Resistant Materials Group developed an automated high-throughput evaluation system. Postdoctoral researcher Dr. Thomas Hoefler and colleagues created a method that dramatically accelerates the generation of process-structure-property datasets, critical for designing high-performance materials in aerospace, energy, and structural engineering.

The method builds on foundational ideas developed by Dr. Takahito Ohmura, Head of the RCSM, and Dr. Toshio Osada, who envisioned multi-indentation and automated SEM workflows to accelerate structural materials research.
 

Automation fundamentally changed how the team approaches alloy characterization. Previously, analyses were limited to basic metrics like phase area fractions and mean precipitate diameters. Now, they evaluate precipitate shapes, inter-precipitate distances, and size distributions across temperature ranges.

The results speak for themselves: 2,400 data points correlating processing conditions, microstructure, and yield strength – gathered in just 13 days.

Traditional tensile testing would take over 200 times longer.

In 2021, Dr. Takahito Ohmura and Dr. Toshio Osada secured funding from Japan's ATLA* to develop multi-indentation combined with 3D SEM imaging. Dr. Ohmura procured ZEISS GeminiSEM 300 and automation infrastructure.

NIMS collaborated with System in Frontier Inc. on the GUI development and with graduate student Eri Nakagawa on workflow testing. Within ZEISS, Dr. Etsuo Maeda contributed to the development of the machine‑learning–based image‑recognition algorithms. This successful work was supported by the National Security Technology Research Promotion Fund of the Acquisition, Technology & Logistics Agency.

Dr. Thomas Hoefler joined as postdoctoral researcher to lead version 2 development – refining workflows and integrating advanced image analysis. Electron microscopy facility manager Dr. Toru Hara provided essential infrastructure support, maintaining NIMS's long-standing ZEISS collaboration. Former member Takuma Kohata also contributed during the early development phases.

*Acquisition, Technology & Logistics Agency in Japan, an organization under the Japanese Ministry of Defense

For NIMS, the impact is clear: a process that once took over seven years can now be completed in under two weeks – freeing up resources, accelerating discovery, and enabling more confident design decisions.
The team’s method supports the development of improved predictive models for phase composition and mechanical properties – especially valuable in aerospace, where complex alloys and extreme temperatures challenge existing databases.
In a study on the nickel-cobalt base superalloy TMP-5002, the system captured measurements at 220 different aging temperatures (647°C to 1,208°C), analyzing nearly one million individual γ′ precipitates. This enabled detailed coarsening kinetics analysis and application of advanced theoretical models with high confidence.

The team is now exploring automated Energy Dispersive X-ray Spectroscopy (EDS) and Electron Backscatter Diffraction (EBSD) to include composition and crystallographic data. They’re also investigating in-situ SEM nanoindentation for high-temperature mechanical testing – critical for aerospace materials that must perform under extreme conditions.

By combining SEM imaging, nanoindentation, and open-source software, the team has built a scalable, high-throughput workflow that delivers consistent, highly correlated data. All analyses are performed on the same sample in a single session, eliminating environmental and operator-related variation – an advantage over traditional multi-sample studies.

The method is applicable to any engineering material accessible to SEM and nanoindentation, making it a powerful tool across the full spectrum of structural materials development.
 

This work builds on earlier research by Dr. Ohmura and Dr. Osada, including the foundational study:
High-throughput evaluation of stress–strain relationships in Ni–Co–Cr ternary systems via indentation testing of diffusion couples, published in Journal of Alloys and Compounds (2022), Volume 918, Article 165829