scholarly journals Image segmentation and analysis for densification mapping of nanoporous gold after nanoindentation

MRS Advances ◽  
2021 ◽  
Author(s):  
Claudia Richert ◽  
Yijuan Wu ◽  
Murilo Hablitzel ◽  
Erica T. Lilleodden ◽  
Norbert Huber
Keyword(s):  
Cross Sections ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Nanoporous Gold ◽  
Sem Images ◽  
Cross Sectional ◽  
Local Thresholding ◽  
Sectional Plane ◽  
Global Thresholding ◽  
Global And Local

AbstractSegmentation of scanning electron microscopy (SEM) images of focused ion beam (FIB) cross-sections through indented regions in nanoporous gold (np-Au) is carried out. A key challenge for image analysis of open porous materials is the appropriate binarization of the pore and gold ligament regions while excluding material lying below the cross-sectional plane. Here, a manual approach to thresholding is compared to global and local approaches. The global thresholding resulted in excessive deviations from the nominal solid fraction, due to a strong gray-scale gradient caused by the tilt angle during imaging and material shadowing. In contrast, the local thresholding approach delivered local solid fractions that were free of global gradients, and delivered a quality comparable to the manual segmentation. The extracted densification profiles vertically below the indenter as well as parallel to the surface showed an exponential-type decay from the indenter tip towards the nominal value of 1 far from the indenter. Graphic abstract

scholarly journals In Situ Delineation Etch Reveals Subtle Detail in SEM Images of Ion Milled Cross Sections Enabling In-Fab 3-D Metrology and Characterization

2000 ◽  
Vol 8 (2) ◽  
pp. 36-39
Author(s):  
Clive Chandler
Keyword(s):  
Sample Preparation ◽  
Cross Sections ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Automated System ◽  
Sem Images ◽  
Difficult Time ◽  
Device Structures ◽  
Wet Etch ◽  
Conventional Sample

Control of layer thickness is critically important in the manufacture of semiconductor devices. Cross-sectioning exposes device structures for direct examination but conventional sample preparation procedures are difficult, time consuming, and grossly destructive. Cross sections created by focused ion beam (FIB) milling are easier, faster, and less destructive but have not offered the clear layer delineation provided by etching in the conventional sample preparation process. A new gas etch capability (Delineation Etch™ from FEI Company) offers results that are equivalent to conventional wet-etch preparations in a fraction of the time from a single, automated system in the fab without destroying the wafer. The new etch process also has application in milling high-aspect-ratio holes to create contacts to buried metal layers, and in deprocessing devices to reveal silicon and polysilicon structures.

FIB Micro-Pillar Sampling of Si Devices and its 3D Observation

2003 ◽  
Author(s):  
T. Yaguchi ◽  
T. Kamino ◽  
T. Ohnishi ◽  
T. Hashimoto ◽  
K. Umemura ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Three Dimensional ◽  
Sampling Technique ◽  
Scanning Transmission Electron Microscope ◽  
Dark Field ◽  
Limiting Factor ◽  
Sem Images ◽  
Cross Sectional ◽  
Scanning Transmission

Abstract A novel technique for three-dimensional structural and elemental analyses using a dedicated focused ion beam (FIB) and scanning transmission electron microscope (STEM) has been developed. The system employs an FIB-STEM compatible sample holder with sample stage rotation mechanism. A piece of sample (micro sample) is extracted from the area to be characterized by the micro-sampling technique [1-3]. The micro sample is then transferred onto the tip of the stage (needle stage) and bonded by FIB assisted metal deposition. STEM observation of the micro sample is carried out after trimming the sample into a micro-pillar 2-5 micron squared in cross-section and 10 -15 micron in length (micro-pillar sample). High angle annular dark field (HAADF) STEM, bright field STEM and secondary electron microscopy (SEM) images are obtained at 200kV resulting in threedimensional and cross sectional representations of the microsample. The geometry of the sample and the needle stage allows observation of the sample from all directions. The specific site can be located for further FIB milling whenever it is required. Since the operator can choose materials for the needle stage, the geometry of the original specimen is not a limiting factor for quantitative energy dispersive X-ray (EDX) analysis.

Scanning Electron Microscopy Observation of Interface Between Single Neurons and Conductive Surfaces

2016 ◽  
Vol 16 (4) ◽  
pp. 3383-3387 ◽  
Author(s):  
Toichiro Goto ◽  
Nahoko Kasai ◽  
Rick Lu ◽  
Roxana Filip ◽  
Koji Sumitomo
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Indium Tin Oxide ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Single Neurons ◽  
Sem Images ◽  
Cross Sectional ◽  
Integrated Devices ◽  
Scanning Electron

Interfaces between single neurons and conductive substrates were investigated using focused ion beam (FIB) milling and subsequent scanning electron microscopy (SEM) observation. The interfaces play an important role in controlling neuronal growth when we fabricate neuron-nanostructure integrated devices. Cross sectional images of cultivated neurons obtained with an FIB/SEM dual system show the clear affinity of the neurons for the substrates. Very few neurons attached themselves to indium tin oxide (ITO) and this repulsion yielded a wide interspace at the neuron-ITO interface. A neuron-gold interface exhibited partial adhesion. On the other hand, a neuron-titanium interface showed good adhesion and small interspaces were observed. These results are consistent with an assessment made using fluorescence microscopy. We expect the much higher spatial resolution of SEM images to provide us with more detailed information. Our study shows that the interface between a single neuron and a substrate offers useful information as regards improving surface properties and establishing neuron-nanostructure integrated devices.

FIB Sample Preparation of Polymer Thin Films on Hard Substrates Using the Shadow-FIB Method

2009 ◽  
Vol 17 (6) ◽  
pp. 20-23 ◽  
Author(s):  
Suhan Kim ◽  
Gao Liu ◽  
Andrew M. Minor
Keyword(s):  
Thin Film ◽  
Cross Sections ◽  
Focused Ion Beam ◽  
Sacrificial Layer ◽  
Ion Beam ◽  
Initial Sample ◽  
Cross Sectional ◽  
Site Specific ◽  
Transmission Electron ◽  
Hard Substrates

Focused ion beam (FIB) instrumentation has proven to be extremely useful for preparing cross-sectional samples for transmission electron microscopy (TEM) investigations. The two most widely used methods involve milling a trench on either side of an electron-transparent window: the “H-bar” and the “lift-out” methods [1]. Although these two methods are very powerful in their versatility and ability to make site-specific TEM samples, they rely on using a sacrificial layer to protect the surface of the sample as well as the removal of a relatively large amount of material, depending on the size of the initial sample. In this article we describe a technique for making thin film cross-sections with the FIB, known as Shadow FIBing, that does not require the use of a sacrificial layer or long milling times [2].

Focused Ion Beam Sample Preparation of Non-Semiconductor Materials

1997 ◽  
Vol 480 ◽  
Author(s):  
M. W. Phaneuf ◽  
N. Rowlands ◽  
G. J. C. Carpenter ◽  
G. Sundaram
Keyword(s):  
Cross Sections ◽  
Automobile Industry ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Semiconductor Industry ◽  
Semiconductor Materials ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Cross Sectional ◽  
Galvannealed Steel

AbstractFocused Ion Beam (FIB) systems have been steadily gaining acceptance as specimen preparation tools in the semiconductor industry. This is largely due to the fact that such instruments are relatively commonplace as failure analysis tools in semiconductor houses, and are commonly used in the preparation of cross-sections for imaging under the ion beam or using an electron beam in an SEM. Additionally, the ease with which cross-sectional TEM specimens of semiconductor devices can be prepared using FIB systems has been well demonstrated. However, this technology is largely unknown outside the semiconductor industry. Relatively few references exist in the literature on the preparation of cross-sectional TEM specimens of non-semiconductor materials by FIB. This paper discusses a specific use of FIB technology in the preparation of cross-sectional TEM specimens of non-semiconductor samples that are difficult to prepare by conventional means. One example of such materials is commercial galvannealed steel sheet that is used to form corrosion resistant auto-bodies for the automobile industry. Cross-sectional TEM specimens of this material have proved difficult and time-intensive to prepare by standard polishing and ion milling techniques due to galvanneal's inherent flaking and powdering difficulties, as well as the different sputtering rates of the various Fe-Zn intermetallic phases present in the galvannealed coatings. TEM results from cross-sectional samples of commercial galvannealed steel coatings prepared by conventional ion milling and FIB techniques are compared to assess image quality, the size of the electron-transparent thin regions that can be readily prepared and the quality of samples produced by both techniques. Specimen preparation times for both techniques are reported.

Image Segmentation for FIB-SEM Serial Sectioning of a Si/C–Graphite Composite Anode Microstructure Based on Preprocessing and Global Thresholding

2019 ◽  
Vol 25 (05) ◽  
pp. 1139-1154
Author(s):  
Dongjae Kim ◽  
Sihyung Lee ◽  
Wooram Hong ◽  
Hyosug Lee ◽  
Seongho Jeon ◽  
...  
Keyword(s):  
High Performance ◽  
Focused Ion Beam ◽  
Low Cost ◽  
Ion Beam ◽  
Lithium Ion ◽  
High Energy ◽  
Sem Images ◽  
Graphite Composite ◽  
Thresholding Method ◽  
Global Thresholding

AbstractThe choice of materials that constitute electrodes and the way they are interconnected, i.e., the microstructure, influences the performance of lithium-ion batteries. For batteries with high energy and power densities, the microstructure of the electrodes must be controlled during their manufacturing process. Moreover, understanding the microstructure helps in designing a high-performance, yet low-cost battery. In this study, we propose a systematic algorithm workflow for the images of the microstructure of anodes obtained from a focused ion beam scanning electron microscope (FIB-SEM). Here, we discuss the typical issues that arise in the raw FIB-SEM images and the corresponding preprocessing methods that resolve them. Next, we propose a Fourier transform-based filter that effectively reduces curtain artifacts. Also, we propose a simple, yet an effective, global-thresholding method to identify active materials and pores in the microstructure. Finally, we reconstruct the three-dimensional structures by concatenating the segmented images. The whole algorithm workflow used in this study is not fully automated and requires user interactions such as choosing the values of parameters and removing shine-through artifacts manually. However, it should be emphasized that the proposed global-thresholding method is deterministic and stable, which results in high segmentation performance for all sectioning images.

Observations of nanoindents via cross-sectional transmission electron microscopy: a survey of deformation mechanisms

2005 ◽  
Vol 461 (2060) ◽  
pp. 2521-2543 ◽  
Author(s):  
S.J Lloyd ◽  
A Castellero ◽  
F Giuliani ◽  
Y Long ◽  
K.K McLaughlin ◽  
...  
Keyword(s):  
Cross Sections ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Deformation Behaviour ◽  
Shear Bands ◽  
Three Dimensional ◽  
Deformation Mechanisms ◽  
Lattice Rotation ◽  
Cross Sectional ◽  
Transmission Electron

Examination of cross-sections of nanoindents with the transmission electron microscope has recently become feasible owing to the development of focused ion beam milling of site-specific electron transparent foils. Here, we discuss the development of this technique for the examination of nanoindents and survey the deformation behaviour in a range of single crystal materials with differing resistances to dislocation flow. The principal deformation modes we discuss, in addition to dislocation flow, are phase transformation (silicon and germanium), twinning (gallium arsenide and germanium at 400 °C), lattice rotations (spinel), shear (spinel), lattice rotations (copper) and lattice rotations and densification (TiN/NbN multilayers). The magnitude of the lattice rotation, about the normal to the foil, was measured at different positions under the indents. Indents in a partially recrystallized metallic glass Mg 66 Ni 20 Nd 14 were also examined. In this case a low-density porous region was formed at the indent tip and evidence of shear bands was also found. Further understanding of indentation deformation will be possible with three-dimensional characterization coupled with modelling which takes account of the variety of competing deformation mechanisms that can occur in addition to dislocation glide. Mapping the lattice rotations will be a particularly useful way to evaluate models of the deformation process.

scholarly journals Enhanced Sample Preparation of Cu Low-k Semiconductors via Mechanical Polishing and Ion Beam Etching

2004 ◽  
Vol 12 (1) ◽  
pp. 41-43
Author(s):  
Shane Roberts ◽  
Daniel Flatoff
Keyword(s):  
Cross Sections ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Dielectric Materials ◽  
Alternative Methods ◽  
Ion Milling ◽  
Cross Sectional ◽  
Ion Beam Etching ◽  
Processing Power ◽  
Materials Used

Modern microelectronics have rapidly decreased in geometry to enhance the speed and processing power of computers. Advanced devices are approaching design rules of sub 0.13 micron in size, and the trend continues at the rate dictated by Moore's Law, Coupled with this reduction in device size, is a change in materials used for producing these devices. Traditional aluminum interconnect metallurgy and oxide dielectric materials are being replaced with copper and low-kmaterials in an effort to continue the trend of shrinking device sizes and higher processing capacities.These changes in materials and device sizes have provided the impetus for alternative methods for producing cross sections. Although focused ion beam instrumentation has been successfully used for preparing cross sections, a combinatorial approach using polishing and argon ion milling has been found to dramatically enhance the ability to produce high quality cross sectional samples in a reasonably short amount of time.

FIB Plan and Side View Cross-Sectional TEM Sample Preparation of Nanostructures

2013 ◽  
Vol 20 (1) ◽  
pp. 133-140 ◽  
Author(s):  
Filip Lenrick ◽  
Martin Ek ◽  
Daniel Jacobsson ◽  
Magnus T. Borgström ◽  
L. Reine Wallenberg
Keyword(s):  
Sample Preparation ◽  
Cross Sections ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Substrate Surface ◽  
Side View ◽  
Transmission Electron Microscopy Analysis ◽  
Cross Sectional ◽  
Transmission Electron ◽  
Electron Microscopy Analysis

AbstractFocused ion beam is a powerful method for cross-sectional transmission electron microscope sample preparation due to being site specific and not limited to certain materials. It has, however, been difficult to apply to many nanostructured materials as they are prone to damage due to extending from the surface. Here we show methods for focused ion beam sample preparation for transmission electron microscopy analysis of such materials, demonstrated on GaAs–GaInP core shell nanowires. We use polymer resin as support and protection and are able to produce cross-sections both perpendicular to and parallel with the substrate surface with minimal damage. Consequently, nanowires grown perpendicular to the substrates could be imaged both in plan and side view, including the nanowire–substrate interface in the latter case. Using the methods presented here we could analyze the faceting and homogeneity of hundreds of adjacent nanowires in a single lamella.

Microstructural Investigation of the Deformation Zone below Nano-Indents in Copper

2007 ◽  
Vol 1049 ◽  
Author(s):  
Martin Rester ◽  
Christian Motz ◽  
Reinhard Pippan
Keyword(s):  
Cross Sections ◽  
Deformation Zone ◽  
Focused Ion Beam ◽  
Electron Backscatter Diffraction ◽  
Shape Change ◽  
Ion Beam ◽  
Dislocation Loops ◽  
Cross Sectional ◽  
Microstructural Investigation ◽  
Experimental Findings

AbstractThe deformation zone below nanoindents in copper single crystals with an <110>{111} orientation is investigated. Using a focused ion beam (FIB) system, cross-sections through the center of the indents were fabricated and subsequently analyzed by means of electron backscatter diffraction (EBSD) technique. Additionally, cross-sectional TEM foils were prepared and examined. Due to changes in the crystal orientation around and beneath the indentations, the plastically deformed zone can be visualized and related to the measured hardness values. Furthermore, the hardness data were analyzed using the Nix-Gao model where a linear relationship was found for H2 vs. 1/hc, but with different slopes for large and shallow indentations. The measured orientation maps indicate that this behavior is presumably caused by a change in the deformation mechanism. On the basis of possible dislocation arrangements, two models are suggested and compared to the experimental findings. The model presented for large imprints is based on dislocation pile-ups similar to the Hall-Petch effect, while the model for shallow indentations uses far-reaching dislocation loops to accommodate the shape change of the imprint.

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