Three-Dimensional Microscopic Elemental Analysis Using an Automated High-Precision Serial Sectioning System

Abstract

Abstract:The elemental composition and microscopic-level shape of inclusions inside industrial materials are considered important factors in fracture analytical studies. In this work, a three-dimensional~3D! microscopic elemental analysis system based on a serial sectioning technique was developed to observe the internal structure of such materials. This 3D elemental mapping system included an X-ray fluorescence analyzer and a highprecision milling machine. Control signals for the X-ray observation process were automatically sent from a data I/O system synchronized with the precision positioning on the milling machine. Composite specimens were used to confirm the resolution and the accuracy of 3D models generated from this system. Each of the two specimens was composed of three metal wires of 0.5 mm diameter braided into a single twisted wire that was placed inside a metal pipe; the pipe was then filled with either epoxy resin or Sn. The milling machine was used to create a mirror-finish cross-sectional surface on these specimens, and elemental analyses were performed. The twisted wire structure was clearly observed in the resulting 3D models. This system enables automated investigation of the 3D internal structure of materials as well as the identification of their elemental components.

An automated three-dimensional internal structure observation system based on high-speed serial sectioning of steel materials

“…Many analyses can be applied to surfaces produced by sectioning process. Since our system features a high-precision positioning device, the system could be used not only for imaging but also for elemental mapping analysis [4] or for micro-hardness measurements on serial sectioning surfaces. The 3D volume 20 models generated from 2D images acquired with this technique can be directly used in mechanical analysis, such as finite elemental analysis.…”

“…On the other hand, destructive serial sectioning was used for the observation of the three-dimensional (3D) internal structure of materials. This method can be combined with other surface analysis techniques such as crystallography and elemental analysis [4]. In destructive serial sectioning, a 3D structural model is constructed from individual two-dimensional (2D) images obtained by continuous sectioning and 5 observation throughout the sample.…”

X-ray dark-field phase-contrast imaging: Origins of the concept to practical implementation and applications

“…3D-ISM was originally devised by a Japanese researcher, T. Higuchi, in 1990. The technique was developed to observe the internal structures of materials, such as biological samples and industrial materials, on a microscopic scale [70,71]. A 3D-ISM system comprises a computed drive cryotome, a high-sensitivity CCD camera, a rewritable laserdisc recorder, and a computer with a graphic workstation [70].…”

“…Images of each cut surface are recorded by a CCD camera and stored in a digital format. After all of the images are captured, a 3D images of the sample is reconstructed by a full-color ray-casting volume-rendering method [70][71][72]. This system enables automated investigation of the 3D internal structure of a sample and is compatible with various imaging techniques including fluorescence imaging and whole-mount staining with clearing.…”

Atomic spectrometry update. Industrial analysis: metals, chemicals and advanced materials

“…About 4% of the pieces were found to be non-compliant with Californian health standards. 31 The milling machine removed precisely measured layers of the material prior to each set of XRF analyses to build a three dimensional elemental picture. 30 Proficiency test samples were analysed using a conventionally calibrated XRF method and then again with a calibration using the Uniquant fundamental parameter software package.…”