The Japan Institute of Physical Chemistry has successfully developed the "Riken Micro Slicer System-003", a continuous section cutting observation system that visualizes a micrometer-scale microstructure. According to this system, it is possible to observe an object which is difficult to observe by X-rays, such as inclusions of several tens of μm inside the steel material. This is the result of a research team centered on the research team of the Bio-infrastructure Construction Team of the Science and Technology Intellectual Property Center, the Assistant Professor of Hokkaido University, Fujisaki Kazuhiro, and the team leader Yokota Yokota.
The failure and fatigue properties of industrial materials depend on stress concentration and local deformation due to the internal structure of the material. It has been known that especially in the environment where the load is repeatedly applied, inclusions, gaps, and grain boundaries and defects in the material may become the starting point for cracking. However, it is unclear what kind of inclusions, inclusions and cracks are inside the material. If the shape and distribution of the inclusions and the extended form of the crack can be observed, the material damage can be ascertained and predicted.
The method of observing the internal structure was taken by X-ray microscopic CT. X-ray micro-CT imaging estimates the internal structure based on the attenuation of X-rays inside the material. In this way, if it is a material that is difficult to penetrate by X-rays, there is a limit in the thickness that can be measured. Therefore, when observing the internal structure of such materials, it is necessary to use a cross-sectional observation method in which a sample is cut, a cross-section is mirror-finished, and observation is performed by a microscope. This observation method obtains three-dimensional data of the internal structure (continuous section method) by observing the surface while cutting the surface a little bit.
However, this method requires labor and time to grind the various sections, and investigation involving multiple sections is difficult. In addition, to overlap the cross-sectional image and make it three-dimensional, it is necessary to correct the positional deviation between the captured images and accurately grasp the depth direction information - the thickness of the grinding. Therefore, it is usually necessary to mark the positioning marks of the respective cross sections and the marks as the grinding depth pointer on the sample cross section. Despite this, it is still difficult to obtain three-dimensional information in terms of accuracy in the μm level.
This study used the three-dimensional internal structure microscope "Riken Micro Slicer System-001/002" developed by the Biomechanical Simulation Research Group. The microscope is specifically designed to observe the internal structure of biological tissues, and repeatedly observe the cut and cross section of the sample to investigate the three-dimensional structure inside the sample. It can be used to observe the hardest biological tissue teeth and bones as well as plastics and metals used as industrial materials. The Riken Micro Slicer System-003 (Figure 1) has been developed.
The new system has less than ±1μm positioning accuracy, so there is no need to correct the position between the captured images. Therefore, mirror processing and microscopic observation of the metal material can be automatically performed between a plurality of sections. The new system introduces a precision cutting technology based on a high-speed rotating spindle, which can observe the internal structure of metal materials such as aluminum alloy and copper at a speed of one minute per section.
In general, single-crystal diamond tools are often used for mirror machining based on precision cutting. However, diamond tools and iron-based materials are difficult to be compatible, and the cutting tool immediately wears the tool, making it difficult to produce the mirror surface required for microscopic observation. Therefore, the new system uses ultrasonic elliptical vibration cutting in the mirror generation of steel materials (the method of moving the tool bit along the elliptical orbit by ultrasonic vibration and cutting, thereby reducing the wear of the cutter head). In this way, the internal structure of high-strength steel such as bearings can be observed.
The team used a new system to observe tens of μm inclusions inside the bearing. The sample cut the bearing into a 3 x 3 x 20 mm prism. Inclusions inside (0.1 to 0.2 mm from the surface layer) were confirmed by ultrasonic flaw detection in advance. The resolution of the new system is 0.8 × 0.8 μm per pixel on the observation surface, and is 2 μm in the depth direction depending on the thickness of the cut (the maximum resolution has been confirmed to be 0.1 × 0.1 × 0.5 μm). When the number of observation sections is 200, it is not necessary to change the tool due to wear or breakage of the cutter head during the cutting process. The mirror processing using the system uses a tool to repeatedly perform the relative reciprocating planing method. By introducing a tool having a large cutter head shape per reciprocating cutting area, each section can be realized in a 3×3 mm observation surface for two minutes. Speed ​​up. In this observation, by three-dimensionally imaging the cross-sectional image and the contour shape of the inclusions, it is possible to see protrusions having a size of several μm and inclusions having small irregularities on the surface (Fig. 2).
This allows the new system to calculate volume and surface area based on digitized shape data. In addition, precision cutting cuts from the surface of the sample at an accurate thickness, so the depth of the inclusions can be known depending on the number of images. By recombining the image, the three-dimensional position of the inclusions, the distance between the plurality of inclusions, and the like can be accurately reproduced.
The cross-section observation method exposes the internal structure to the surface, so it can be used not only for microscopic observation but also for structural performance investigation. If the elemental analysis of the inclusions and the orientation survey of the crystal grains are used together with the cross-sectional observation, the non-uniformity distribution inside the material can be accurately obtained and reproduced in a computer. In addition, it can be applied to the calculation of shape parameters such as volume, surface area and aspect ratio according to the 3D model, and the mechanical simulation of the VCAD system being developed by Riken. Therefore, it is expected that the internal stress analysis of the material can be realized by computer simulation. . In the future, in addition to the form of inclusions, the distribution of cracks and the distribution of internal properties will be investigated in detail, and it is expected to develop new technologies that can resolve the phenomenon of material damage that has not been clarified before.
The failure and fatigue properties of industrial materials depend on stress concentration and local deformation due to the internal structure of the material. It has been known that especially in the environment where the load is repeatedly applied, inclusions, gaps, and grain boundaries and defects in the material may become the starting point for cracking. However, it is unclear what kind of inclusions, inclusions and cracks are inside the material. If the shape and distribution of the inclusions and the extended form of the crack can be observed, the material damage can be ascertained and predicted.
The method of observing the internal structure was taken by X-ray microscopic CT. X-ray micro-CT imaging estimates the internal structure based on the attenuation of X-rays inside the material. In this way, if it is a material that is difficult to penetrate by X-rays, there is a limit in the thickness that can be measured. Therefore, when observing the internal structure of such materials, it is necessary to use a cross-sectional observation method in which a sample is cut, a cross-section is mirror-finished, and observation is performed by a microscope. This observation method obtains three-dimensional data of the internal structure (continuous section method) by observing the surface while cutting the surface a little bit.
However, this method requires labor and time to grind the various sections, and investigation involving multiple sections is difficult. In addition, to overlap the cross-sectional image and make it three-dimensional, it is necessary to correct the positional deviation between the captured images and accurately grasp the depth direction information - the thickness of the grinding. Therefore, it is usually necessary to mark the positioning marks of the respective cross sections and the marks as the grinding depth pointer on the sample cross section. Despite this, it is still difficult to obtain three-dimensional information in terms of accuracy in the μm level.
This study used the three-dimensional internal structure microscope "Riken Micro Slicer System-001/002" developed by the Biomechanical Simulation Research Group. The microscope is specifically designed to observe the internal structure of biological tissues, and repeatedly observe the cut and cross section of the sample to investigate the three-dimensional structure inside the sample. It can be used to observe the hardest biological tissue teeth and bones as well as plastics and metals used as industrial materials. The Riken Micro Slicer System-003 (Figure 1) has been developed.
The new system has less than ±1μm positioning accuracy, so there is no need to correct the position between the captured images. Therefore, mirror processing and microscopic observation of the metal material can be automatically performed between a plurality of sections. The new system introduces a precision cutting technology based on a high-speed rotating spindle, which can observe the internal structure of metal materials such as aluminum alloy and copper at a speed of one minute per section.
In general, single-crystal diamond tools are often used for mirror machining based on precision cutting. However, diamond tools and iron-based materials are difficult to be compatible, and the cutting tool immediately wears the tool, making it difficult to produce the mirror surface required for microscopic observation. Therefore, the new system uses ultrasonic elliptical vibration cutting in the mirror generation of steel materials (the method of moving the tool bit along the elliptical orbit by ultrasonic vibration and cutting, thereby reducing the wear of the cutter head). In this way, the internal structure of high-strength steel such as bearings can be observed.
The team used a new system to observe tens of μm inclusions inside the bearing. The sample cut the bearing into a 3 x 3 x 20 mm prism. Inclusions inside (0.1 to 0.2 mm from the surface layer) were confirmed by ultrasonic flaw detection in advance. The resolution of the new system is 0.8 × 0.8 μm per pixel on the observation surface, and is 2 μm in the depth direction depending on the thickness of the cut (the maximum resolution has been confirmed to be 0.1 × 0.1 × 0.5 μm). When the number of observation sections is 200, it is not necessary to change the tool due to wear or breakage of the cutter head during the cutting process. The mirror processing using the system uses a tool to repeatedly perform the relative reciprocating planing method. By introducing a tool having a large cutter head shape per reciprocating cutting area, each section can be realized in a 3×3 mm observation surface for two minutes. Speed ​​up. In this observation, by three-dimensionally imaging the cross-sectional image and the contour shape of the inclusions, it is possible to see protrusions having a size of several μm and inclusions having small irregularities on the surface (Fig. 2).
This allows the new system to calculate volume and surface area based on digitized shape data. In addition, precision cutting cuts from the surface of the sample at an accurate thickness, so the depth of the inclusions can be known depending on the number of images. By recombining the image, the three-dimensional position of the inclusions, the distance between the plurality of inclusions, and the like can be accurately reproduced.
The cross-section observation method exposes the internal structure to the surface, so it can be used not only for microscopic observation but also for structural performance investigation. If the elemental analysis of the inclusions and the orientation survey of the crystal grains are used together with the cross-sectional observation, the non-uniformity distribution inside the material can be accurately obtained and reproduced in a computer. In addition, it can be applied to the calculation of shape parameters such as volume, surface area and aspect ratio according to the 3D model, and the mechanical simulation of the VCAD system being developed by Riken. Therefore, it is expected that the internal stress analysis of the material can be realized by computer simulation. . In the future, in addition to the form of inclusions, the distribution of cracks and the distribution of internal properties will be investigated in detail, and it is expected to develop new technologies that can resolve the phenomenon of material damage that has not been clarified before.
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