scholarly journals Interlaboratory Measurements of Contiguity in WC-Co Hardmetals

Metals ◽  
2019 ◽  
Vol 9 (3) ◽  
pp. 328 ◽  
Author(s):  
Ken Mingard ◽  
Bryan Roebuck
Keyword(s):  
High Resolution ◽  
Grain Boundaries ◽  
Electron Backscatter Diffraction ◽  
Ion Beam ◽  
Recent Analysis ◽  
Polished Surface ◽  
Binder Phase ◽  
Sem Images ◽  
Significant Difference ◽  
Etched Surface

The contiguity of a hardmetal is a measure of the proportion of the carbide grain boundaries that are in direct contact with other carbide grain boundaries. Recent analysis of data available in the literature shows a large scatter in results and a significant difference in values measured from scanning electron microscope (SEM) images and from electron backscatter diffraction (EBSD) mapping. An interlaboratory exercise has been carried out with the measurement of a range of WC-Co hardmetal grades. For each grade, SEM images were acquired from both an etched surface and an ion beam polished surface and EBSD maps with two different processing routes. These maps and images were provided to the participants for measurement to eliminate variability from sample preparation and image acquisition. It was shown that measurement of contiguity from EBSD maps is likely to lead to an overestimation of contiguity, largely because EBSD maps do not have the resolution of SEM images to identify small binder phase regions between WC grains. Ion beam polishing combined with backscattered electron imaging was found to provide the best images of the microstructure to underpin a confident measurement of contiguity. However, high resolution SEM images of etched surfaces gave values close to those from ion beam polished samples so it is recommended that, as etching is much more widely available, high-resolution imaging of a lightly etched WC surface should be promoted as the preferred method for measurement of contiguity, in combination with backscattered imaging where possible. Even with good images, variation between operators can give uncertainties of approximately ±10%.

Implementing Transmission Electron Backscatter Diffraction for Atom Probe Tomography

2016 ◽  
Vol 22 (3) ◽  
pp. 583-588 ◽  
Author(s):  
Katherine P. Rice ◽  
Yimeng Chen ◽  
Ty J. Prosa ◽  
David J. Larson
Keyword(s):  
Grain Boundary ◽  
Grain Boundaries ◽  
Atom Probe Tomography ◽  
Focused Ion Beam ◽  
Electron Backscatter Diffraction ◽  
Ion Beam ◽  
Atom Probe ◽  
Specimen Preparation ◽  
Inconel 600 ◽  
Transmission Electron

AbstractThere are advantages to performing transmission electron backscattering diffraction (tEBSD) in conjunction with focused ion beam-based specimen preparation for atom probe tomography (APT). Although tEBSD allows users to identify the position and character of grain boundaries, which can then be combined with APT to provide full chemical and orientation characterization of grain boundaries, tEBSD can also provide imaging information that improves the APT specimen preparation process by insuring proper placement of the targeted grain boundary within an APT specimen. In this report we discuss sample tilt angles, ion beam milling energies, and other considerations to optimize Kikuchi diffraction pattern quality for the APT specimen geometry. Coordinated specimen preparation and analysis of a grain boundary in a Ni-based Inconel 600 alloy is used to illustrate the approach revealing a 50° misorientation and trace element segregation to the grain boundary.

High-resolution EM study of submicrometer-grained Al-Mg solid solution alloys

1995 ◽  
Vol 53 ◽  
pp. 524-525
Author(s):  
Z. Horita ◽  
D. J. Smith ◽  
M. Furukawa ◽  
M. Nemoto ◽  
R. Z. Valiev ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
High Resolution ◽  
Grain Boundaries ◽  
Energy State ◽  
High Energy ◽  
Grain Structure ◽  
Boundary Structure ◽  
Solid Solution Alloy ◽  
Average Grain Size

It is possible to produce metallic materials with submicrometer-grained (SMG) structures by imposing an intense plastic strain under quasi-hydrostatic pressure. Studies using conventional transmission electron microscopy (CTEM) showed that many grain boundaries in the SMG structures appeared diffuse in nature with poorly defined transition zones between individual grains. The implication of the CTEM observations is that the grain boundaries of the SMG structures are in a high energy state, having non-equilibrium character. It is anticipated that high-resolution electron microscopy (HREM) will serve to reveal a precise nature of the grain boundary structure in SMG materials. A recent study on nanocrystalline Ni and Ni3Al showed lattice distortion and dilatations in the vicinity of the grain boundaries. In this study, HREM observations are undertaken to examine the atomic structure of grain boundaries in an SMG Al-based Al-Mg alloy.An Al-3%Mg solid solution alloy was subjected to torsion straining to produce an equiaxed grain structure with an average grain size of ~0.09 μm.

High-resolution electron microscopy of nanostructured materials

1995 ◽  
Vol 53 ◽  
pp. 172-173
Author(s):  
M. José-Yacamán
Keyword(s):  
Electron Microscopy ◽  
High Resolution ◽  
Grain Boundaries ◽  
Nanostructured Materials ◽  
High Resolution Electron Microscopy ◽  
Hrem Image ◽  
Small Particles ◽  
Resolution Electron ◽  
Nanophase Materials

Electron microscopy is a fundamental tool in materials characterization. In the case of nanostructured materials we are looking for features with a size in the nanometer range. Therefore often the conventional TEM techniques are not enough for characterization of nanophases. High Resolution Electron Microscopy (HREM), is a key technique in order to characterize those materials with a resolution of ~ 1.7A. High resolution studies of metallic nanostructured materials has been also reported in the literature. It is concluded that boundaries in nanophase materials are similar in structure to the regular grain boundaries. That work therefore did not confirm the early hipothesis on the field that grain boundaries in nanostructured materials have a special behavior. We will show in this paper that by a combination of HREM image processing, and image calculations, it is possible to prove that small particles and coalesced grains have a significant surface roughness, as well as large internal strain.

Recent applications of TEM to the study of interfaces

1990 ◽  
Vol 48 (4) ◽  
pp. 308-309
Author(s):  
C. Barry Carter
Keyword(s):  
High Resolution ◽  
Sample Preparation ◽  
Grain Boundaries ◽  
Diffuse Scattering ◽  
Imaging Techniques ◽  
Amorphous Material ◽  
Contrast Imaging ◽  
Current State ◽  
Actual Nature ◽  
High Resolution Images

This paper will review the current state of understanding of interface structure and highlight some of the future needs and problems which must be overcome. The study of this subject can be separated into three different topics: 1) the fundamental electron microscopy aspects, 2) material-specific features of the study and 3) the characteristics of the particular interfaces. The two topics which are relevant to most studies are the choice of imaging techniques and sample preparation. The techniques used to study interfaces in the TEM include high-resolution imaging, conventional diffraction-contrast imaging, and phase-contrast imaging (Fresnel fringe images, diffuse scattering). The material studied affects not only the characteristics of the interfaces (through changes in bonding, etc.) but also the method used for sample preparation which may in turn have a significant affect on the resulting image. Finally, the actual nature and geometry of the interface must be considered. For example, it has become increasingly clear that the plane of the interface is particularly important whenever at least one of the adjoining grains is crystalline.A particularly productive approach to the study of interfaces is to combine different imaging techniques as illustrated in the study of grain boundaries in alumina. In this case, the conventional imaging approach showed that most grain boundaries in ion-thinned samples are grooved at the grain boundary although the extent of this grooving clearly depends on the crystallography of the surface. The use of diffuse scattering (from amorphous regions) gives invaluable information here since it can be used to confirm directly that surface grooving does occur and that the grooves can fill with amorphous material during sample preparation (see Fig. 1). Extensive use of image simulation has shown that, although information concerning the interface can be obtained from Fresnel-fringe images, the introduction of artifacts through sample preparation cannot be lightly ignored. The Fresnel-fringe simulation has been carried out using a commercial multislice program (TEMPAS) which was intended for simulation of high-resolution images.

“Cavity” formation in superplastically deformed aluminium alloys

1990 ◽  
Vol 48 (4) ◽  
pp. 958-959
Author(s):  
A. Cziráki ◽  
E. Ková-csetényi ◽  
T. Torma ◽  
T. Turmezey
Keyword(s):  
Grain Boundaries ◽  
Aluminium Alloys ◽  
Superplastic Deformation ◽  
Volume Fraction ◽  
Superplastic Forming ◽  
Polished Surface ◽  
Cavity Formation ◽  
Stress Concentrations ◽  
Electron Microscopic ◽  
Commercial Aluminium

It is known that the formation of cavities during superplastic deformation can be correlated with the development of stress concentrations at irregularities along grain boundaries such as particles, ledges and triple points. In commercial aluminium alloys Al-Fe-Si particles or other coarse constituents may play an important role in cavity formation.Cavity formation during superplastic deformation was studied by optical metallography and transmission scanning electron microscopic investigations on Al-Mg-Si and Al-Mg-Mn alloys. The structure of particles was characterized by selected area diffraction and X-ray micro analysis. The volume fraction of “voids” was determined on mechanically polished surface.It was found by electron microscopy that strongly deformed regions are formed during superplastic forming at grain boundaries and around coarse particles.According to electron diffraction measurements these areas consist of small micro crystallized regions. See Fig.l.Comparing the volume fraction and morphology of cavities found by optical microscopy a good correlation was established between that of micro crystalline regions.

FIB Enhancement of Mechanically Polished Cross-sections

2019 ◽  
Author(s):  
Becky Holdford
Keyword(s):  
Electron Microscope ◽  
High Resolution ◽  
Scanning Electron Microscope ◽  
Cross Sections ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
High Resolution Imaging ◽  
Chemical Attack ◽  
Resolution Imaging ◽  
Scanning Electron

Abstract On mechanically polished cross-sections, getting a surface adequate for high-resolution imaging is sometimes beyond the analyst’s ability, due to material smearing, chipping, polishing media chemical attack, etc.. A method has been developed to enable the focused ion beam (FIB) to re-face the section block and achieve a surface that can be imaged at high resolution in the scanning electron microscope (SEM).

The Novel Dopant Profile Inspection Methodology by FIB

2010 ◽  
Author(s):  
Po Fu Chou ◽  
Li Ming Lu
Keyword(s):  
High Resolution ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Real Sample ◽  
Physical Analysis ◽  
The Novel ◽  
High Contrast ◽  
Dopant Profile ◽  
P Type

Abstract Dopant profile inspection is one of the focused ion beam (FIB) physical analysis applications. This paper presents a technique for characterizing P-V dopant regions in silicon by using a FIB methodology. This technique builds on published work for backside FIB navigation, in which n-well contrast is observed. The paper demonstrates that the technique can distinguish both n- and p-type dopant regions. The capability for imaging real sample dopant regions on current fabricated devices is also demonstrated. SEM DC and FIB DC are complementary methodologies for the inspection of dopants. The advantage of the SEM DC method is high resolution and the advantage of FIB DC methodology is high contrast, especially evident in a deep N-well region.

Cross Section Analysis of Cu Filled TSVs Based on High Throughput Plasma-FIB Milling

2012 ◽  
Author(s):  
Frank Altmann ◽  
Jens Beyersdorfer ◽  
Jan Schischka ◽  
Michael Krause ◽  
German Franz ◽  
...  
Keyword(s):  
High Resolution ◽  
Cross Section ◽  
High Throughput ◽  
Cross Sections ◽  
Electron Backscatter Diffraction ◽  
Grain Structure ◽  
Electron Backscatter ◽  
Section Surface ◽  
Backscatter Diffraction ◽  
Section Analysis

Abstract In this paper the new Vion™ Plasma-FIB system, developed by FEI, is evaluated for cross sectioning of Cu filled Through Silicon Via (TSV) interconnects. The aim of the study presented in this paper is to evaluate and optimise different Plasma-FIB (P-FIB) milling strategies in terms of performance and cross section surface quality. The sufficient preservation of microstructures within cross sections is crucial for subsequent Electron Backscatter Diffraction (EBSD) grain structure analyses and a high resolution interface characterisation by TEM.

scholarly journals Revealing Inflammatory Indications Induced by Titanium Alloy Wear Debris in Periprosthetic Tissue by Label-Free Correlative High-Resolution Ion, Electron and Optical Microspectroscopy

Materials ◽  
2021 ◽  
Vol 14 (11) ◽  
pp. 3048
Author(s):  
Rok Podlipec ◽  
Esther Punzón-Quijorna ◽  
Luka Pirker ◽  
Mitja Kelemen ◽  
Primož Vavpetič ◽  
...  
Keyword(s):  
Titanium Alloy ◽  
High Resolution ◽  
Wear Debris ◽  
Ion Beam ◽  
Quantitative Measure ◽  
Label Free ◽  
Periprosthetic Tissue ◽  
Correlative Microscopy ◽  
X Ray ◽  
Tissue Reactions

The metallic-associated adverse local tissue reactions (ALTR) and events accompanying worn-broken implant materials are still poorly understood on the subcellular and molecular level. Current immunohistochemical techniques lack spatial resolution and chemical sensitivity to investigate causal relations between material and biological response on submicron and even nanoscale. In our study, new insights of titanium alloy debris-tissue interaction were revealed by the implementation of label-free high-resolution correlative microscopy approaches. We have successfully characterized its chemical and biological impact on the periprosthetic tissue obtained at revision surgery of a fractured titanium-alloy modular neck of a patient with hip osteoarthritis. We applied a combination of photon, electron and ion beam micro-spectroscopy techniques, including hybrid optical fluorescence and reflectance micro-spectroscopy, scanning electron microscopy (SEM), Energy-dispersive X-ray Spectroscopy (EDS), helium ion microscopy (HIM) and micro-particle-induced X-ray emission (micro-PIXE). Micron-sized wear debris were found as the main cause of the tissue oxidative stress exhibited through lipopigments accumulation in the nearby lysosome. This may explain the indications of chronic inflammation from prior histologic examination. Furthermore, insights on extensive fretting and corrosion of the debris on nm scale and a quantitative measure of significant Al and V release into the tissue together with hydroxyapatite-like layer formation particularly bound to the regions with the highest Al content were revealed. The functional and structural information obtained at molecular and subcellular level contributes to a better understanding of the macroscopic inflammatory processes observed in the tissue level. The established label-free correlative microscopy approach can efficiently be adopted to study any other clinical cases related to ALTR.

scholarly journals Microscopy Methods for Biofilm Imaging: Focus on SEM and VP-SEM Pros and Cons

Biology ◽  
2021 ◽  
Vol 10 (1) ◽  
pp. 51
Author(s):  
Michela Relucenti ◽  
Giuseppe Familiari ◽  
Orlando Donfrancesco ◽  
Maurizio Taurino ◽  
Xiaobo Li ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Ion Beam ◽  
Ruthenium Red ◽  
Variable Pressure ◽  
Sem Images ◽  
Advantages And Disadvantages ◽  
Pros And Cons ◽  
Microscopy Techniques ◽  
Scanning Electron

Several imaging methodologies have been used in biofilm studies, contributing to deepening the knowledge on their structure. This review illustrates the most widely used microscopy techniques in biofilm investigations, focusing on traditional and innovative scanning electron microscopy techniques such as scanning electron microscopy (SEM), variable pressure SEM (VP-SEM), environmental SEM (ESEM), and the more recent ambiental SEM (ASEM), ending with the cutting edge Cryo-SEM and focused ion beam SEM (FIB SEM), highlighting the pros and cons of several methods with particular emphasis on conventional SEM and VP-SEM. As each technique has its own advantages and disadvantages, the choice of the most appropriate method must be done carefully, based on the specific aim of the study. The evaluation of the drug effects on biofilm requires imaging methods that show the most detailed ultrastructural features of the biofilm. In this kind of research, the use of scanning electron microscopy with customized protocols such as osmium tetroxide (OsO4), ruthenium red (RR), tannic acid (TA) staining, and ionic liquid (IL) treatment is unrivalled for its image quality, magnification, resolution, minimal sample loss, and actual sample structure preservation. The combined use of innovative SEM protocols and 3-D image analysis software will allow for quantitative data from SEM images to be extracted; in this way, data from images of samples that have undergone different antibiofilm treatments can be compared.

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