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Calibration of High-Resolution X-Ray Tomography With Atomic Force Microscopy
A R Kalukin1, B Winn2, Y Wang2
1Rensselaer Polytechnic Institute, Troy, NY 12180-3590; National Institute of Standards and Technology, Gaithersburg, MD 20899-8410.
Summary
This study introduces a novel calibration method for nanoscale 3D imaging using scanning transmission x-ray microscopy (STXM). The new technique accurately calibrates STXM tomography images with atomic force microscopy and scanning electron microscopy, overcoming previous limitations.
Area of Science:
- Materials Science
- Nanotechnology
- X-ray Imaging
Background:
- Scanning transmission x-ray microscopy (STXM) achieves nanoscale resolution (40 nm) for 2D imaging of thin films.
- Calibration of 3D tomographic images from STXM data at this scale presents unique challenges not seen in larger-scale X-ray tomography.
- Existing calibration methods like optical imaging are insufficient due to the small feature sizes, and higher-resolution methods like atomic force microscopy (AFM) are destructive and provide surface-only information.
Purpose of the Study:
- To develop and describe a novel procedure for calibrating 3D tomographic images obtained using STXM.
- To overcome the limitations of existing calibration methods, particularly the inability to use optical imaging and the destructive nature of AFM.
- To achieve accurate calibration by correlating STXM tomography data with high-resolution surface imaging techniques.
Main Methods:
- A germanium star-shaped pattern was imaged using STXM at a synchrotron.
- Nineteen high-resolution 2D projection images were acquired and reconstructed into a 3D tomographic image.
- The STXM tomography data was calibrated against images obtained from atomic force microscopy (AFM) and scanning electron microscopy (SEM) of the same sample.
Main Results:
- Features as small as 40 nm were resolved in 2D STXM images and 80 nm in the 3D reconstructed tomographic image.
- Transverse length scales derived from AFM, SEM, X-ray transmission, and tomographic reconstruction agreed within 10 nm.
- The sample thickness calculated from projection images (51 ± 15 nm) showed good agreement with the tomographic reconstruction (80 ± 52 nm), within two standard deviations.
Conclusions:
- The developed procedure successfully calibrates STXM tomography images at the nanoscale.
- This method overcomes limitations of previous techniques, enabling more accurate 3D nanoscale imaging.
- The results demonstrate the feasibility of high-resolution 3D reconstruction and calibration for STXM, advancing nanoscale imaging capabilities.

