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Sample preparation toward seamless 3D imaging technique from micrometer to nanometer scale.

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  • 1Department of Geology and Mineralogy, Graduate School of Science, Kyoto University 606-8502 Kitashirakawa Oiwakecho, Kyoto, Japan.

Microscopy (Oxford, England)
|November 1, 2014
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Summary

This study introduces a novel sample holder and preparation method for advanced 3D imaging, enabling detailed visualization of microstructures in quartz using synchrotron-XCT, FIB-SEM, and TEMT techniques.

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Area of Science:

  • Materials Science and Engineering
  • Geology and Earth Sciences
  • Nanotechnology and Microscopy

Background:

  • Three-dimensional (3D) imaging techniques like X-ray computed tomography (XCT), serial sectioning, transmission electron microtomography (TEMT), and 3D atom probe (3DAP) are crucial for visualizing internal structures.
  • Obtaining correlative 3D data from multiple advanced imaging techniques for the same sample area presents significant methodological challenges.
  • Precise sample manipulation and holder design are critical for high-resolution 3D analysis, especially for delicate samples like those containing fluid inclusions.

Purpose of the Study:

  • To develop and report a common sample holder and an improved TEM tomography retainer for correlative 3D imaging.
  • To establish a sample preparation method using focused ion beam (FIB) for serial sectioning and high-resolution 3D analysis.
  • To demonstrate the capability of obtaining integrated 3D images from synchrotron-XCT (SR-XCT), FIB-SEM, and TEMT of quartz samples with fluid inclusions.

Main Methods:

  • Fabrication of a common sample holder using a tungsten needle and copper pipe, with electropolishing for needle preparation.
  • Micro-sampling of quartz with fluid inclusions using a focused ion beam (FIB) system, followed by platinum deposition for mounting.
  • Correlative imaging using SR-XCT, FIB-SEM serial sectioning, and TEMT, with specialized sample preparation for each technique, including FIB milling for TEMT specimens.

Main Results:

  • Successful acquisition of 3D images from SR-XCT (voxel size 50-80 nm, resolution ~200 nm), FIB-SEM, and TEMT of quartz samples.
  • Demonstration of FIB-XCT's ability to precisely target specific sample areas for subsequent high-resolution imaging.
  • TEMT successfully identified fluid inclusions (20-100 nm) in quartz that were undetectable by FIB-XCT, showcasing enhanced resolution and capability.

Conclusions:

  • The developed common sample holder and TEM retainer facilitate correlative 3D imaging across multiple advanced microscopy techniques.
  • The FIB-based sample preparation method enables precise targeting and serial sectioning for high-resolution 3D reconstruction.
  • This integrated approach significantly enhances the ability to visualize and analyze microstructures, such as fluid inclusions, within geological samples.