The application of scanning electron microscopy to bulk devices. Part 1 - Gunn diodes
Feasibility study of scanning electron microscopy to diagnose properties of small Gunn diodes
SEARCH · Engineering Papers
Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.
Feasibility study of scanning electron microscopy to diagnose properties of small Gunn diodes
Nitrogen vacancy (NV)-containing nanodiamonds are widely used in quantum sensing applications due to their high sensitivity to magnetic fields, relatively low cost, and ability to be initialized, manipulated, and read out at room temperature. Quantum sensing techniques such as optically detected magnetic resonance (ODMR) and spin relaxometry have exploited the sensitivity of the NV nanodiamonds to magnetic fields to detect a range of analytes, such as pH, metal ions, and biomolecules. However, diversifying the sensing targets accessible by NV diamond quantum sensors typically requires careful engineering of the diamond surface chemistry with stimuli-responsive functional groups. Here, a simple protocol for coating NV nanodiamonds with the zeolitic imidazole framework 8 (ZIF-8), a widely used metal-organic framework, is presented. ZIF-8 is a highly porous material that has been used as a selective sensor for gasses, metal ions, and other analytes. The material is well-characterized by x-ray diffraction, transmission electron microscopy, scanning electron microscopy, x-ray photoelectron spectroscopy, and luminescence spectroscopy. Encapsulation of NV nanodiamonds with a porous scaffold such as ZIF-8 provides a promising method for improving the selectivity for the quantum sensing of various analytes. Importantly, the ZIF-8 coating does not impact the luminescence properties of the NV diamond, which is a key readout in ODMR and spin relaxometry sensing approaches. Indeed, the ODMR spectra with and without the ZIF-8 shell is nearly identical. Moreover, the ZIF-8 coating increases the longitudinal spin relaxation time of the NV nanodiamond by a factor of 4 relative to aggregated diamond, a desirable outcome for spin relaxation-based quantum sensing. Metal-organic framework composites with nanodiamonds thus are an exciting strategy for enhancing NV nanodiamond performance in applications such as quantum sensing and quantum-enhanced nuclear magnetic resonance spectroscopy.
The mechanical and thermal conductivity properties of two composite elastomers were studied. Styrene–butadiene rubber (SBR) filled with functionalized graphene oxide (GO) and silica nanofibers, and styrene–butadiene–styrene (SBS) block copolymers filled with graphene oxide. For the SBR composites, GO fillers with two different surface functionalities were synthesized (cysteamine and dodecylamine) and dispersed in the SBR using mechanical and liquid mixing techniques. The hydrophilic cysteamine-based GO fillers were dispersed in the SBR by mechanical mixing, whereas the hydrophobic dodecylamine-based GO fillers were dispersed in the SBR by liquid mixing. Silica nanofibers (SnFs) were fabricated by electrospinning a sol–gel precursor solution. The surface chemistry of the functionalized fillers was studied in detail. The properties of the composites and the synergistic improvements between the GO and SnFs are presented. For the SBS composites, GO fillers were dispersed in the SBS elastomer at several weight percent loadings using liquid mixing. Characterization of the filler material and the composite elastomers was performed using x-ray photoelectron spectroscopy, x-ray diffraction, transmission electron microscopy, scanning electron microscopy, thermogravimetric analysis, dynamic mechanical analysis, tensile testing, nanoindentation, thermal conductivity and abrasion testing.
Methods for analyzing atmospheric aerosols and particulate contaminants from natural and industrial sources are briefly described. Their development was spurred by interest in cosmic dust investigations. These methods make it possible to analyze individual particles ranging in size from 0.01 to 1000 microns for elemental and mineralogical content. The described methods include transmission electron microscopy, scanning electron microscopy, electron probe microanalysis, X-ray diffraction, optical mineralogy, and density measurement.
Examination of Holocene Bahamian ooelites by scanning electron and light microscopy has revealed the morphology and orientation of aragonite crystals in the lamellar ooelitic envelope, and their modification by the boring activities of endolithic algae. The voids produced by these algae are found in progressive stages of being lined and filled with precipitated microcrystalline aragonite, which is similar to the process of micrite envelope formation in molluscan and other skeletal carbonate grains.
Optical and scanning electron microscopy, scanning electron microprobes and energy dispersion techniques were applied in an analysis of six siliceous glass spheres, five siliceous glass-bonded agglutinates and one breccia fragment from Luna 20 sample 22003. It is theorized that local meteor impact processes might have been responsible for the formation of most of the glass spheres and that the impacts of relatively high velocity particles might have been responsible for the craters observed on the surfaces of the spheres. The concentrations of iron spherules on the surfaces of the glass spheres were generally lower than in similar Apollo 11 and 12 glass spheres.
Damage scar volume measurements taken from like metal fretting pairs combined with scanning electron microscopy observations showed that three sequentially operating mechanisms result in the fretting of titanium, Monel-400, and cobalt - 25-percent molybdenum. Initially, adhesion and plastic deformation of the surface played an important role. This was followed after a few hundred cycles by a fatigue mechanism which produced spall-like pits in the damage scar. Finally, a combination of oxidation and abrasion by debris particles became most significant. Damage scar measurements made on several elemental metals after 600,000 fretting cycles suggested that the ratio of oxide hardness to metal hardness was a measure of the susceptibility of a metal to progressive damage by fretting.
Damage scar volume measurements taken from like metal fretting pairs, combined with scanning electron microscopy observations, showed that three sequentially operating mechanisms result in the fretting of titanium, Monel-400, and cobalt-25% molybdenum. Initially, adhesion and plastic deformation on the surface played an important role. This was followed after a few hundred cycles by a fatigue mechanism, producing spall-like pits in the damage scar. Finally, an oxidation-related mechanism became most significant. Damage scar measurements made on several elemental metals after 600,000 fretting cycles suggested that the ratio of oxide hardness to metal hardness was a measure of the susceptibility of a metal to progressive damage by fretting.
Organic–inorganic perovskites are an emerging class of photovoltaic materials. Despite achieving power conversion efficiencies surpassing 26%, the challenge of perovskite stability including degradation during exposure to operational conditions such as light, heat, humidity, water, oxygen, and electric fields is well known. Related, perovskite instability has limited high-resolution electron imaging and characterization techniques that can be used for understanding degradation mechanisms. Furthermore, we demonstrate perovskite device cross-section preparation using mechanical polishing in a water-free environment with cryogenic Ar ion milling. Scanning electron microscopy was then used in both backscattered electron and secondary electron imaging modes to obtain information about layer structure, grain aggregate structure, and compositional heterogeneity. Monte Carlo CASINO simulations inform optimum beam conditions and image acquisition parameters and the effects of accelerating voltage, dwell times, and frame averaging for practical image acquisition are reported.
Despite many studies of subsurface imaging of carbon nanotube (CNT)-polymer composites via scanning electron microscopy (SEM), significant controversy exists concerning the imaging depth and contrast mechanisms. We studied CNT-polyimide composites and, by threedimensional reconstructions of captured stereo-pair images, determined that the maximum SEM imaging depth was typically hundreds of nanometers. The contrast mechanisms were investigated over a broad range of beam accelerating voltages from 0.3 to 30 kV, and ascribed to modulation by embedded CNTs of the effective secondary electron (SE) emission yield at the polymer surface. This modulation of the SE yield is due to non-uniform surface potential distribution resulting from current flows due to leakage and electron beam induced current. The importance of an external electric field on SEM subsurface imaging was also demonstrated. The insights gained from this study can be generally applied to SEM nondestructive subsurface imaging of conducting nanostructures embedded in dielectric matrices such as graphene-polymer composites, silicon-based single electron transistors, high resolution SEM overlay metrology or e-beam lithography, and have significant implications in nanotechnology.
The dissociation supernatant (DS) isolated by disaggregating Strongylocentrotus purpuratus blastulae in calcium- and magnesium-free seawater specifically promotes reaggregation of S. purpuratus blastula cells. The purpose of this study was to use scanning electron microscopy to examine the gross morphology of aggregates formed in the presence of DS to see if it resembles adhesion in partially dissociated blastulae. A new reaggregation procedure developed here, using large volumes of cell suspension and a large diameter of rotation, was utilized to obtain sufficient quantities of aggregates for scanning electron microscopy. The results indicate that aggregates formed in the presence of DS resemble partially dissociated intact embryos in terms of the direct cell-cell adhesion observed. DS did not cause aggregation to form as a result of the entrapment of cells in masses of extracellular material. These studies provide the groundwork for further studies using transmission electron microscopy to more precisely define the adhesive contacts made by cells in the presence of the putative adhesion molecules present in DS.
The compound, 2-(2,4-dinitrobenzyl) pyridine, was synthesized in the laboratory; an introductory level electron microscopy study of the macro-crystalline structure was conducted using the scanning electron microscope (SEM). The structure of these crystals was compared with the macrostructure of the crystal of 2-(2,4-dinitrobenzyl) pyridinium bromide, the hydrobromic salt of the compound which was also synthesized in the laboratory. A scanning electron microscopy crystal study was combined with a study of the principle of the electron microscope.
BeO whiskers formation on burning Be droplets surface using scanning electron microscopy, noting temperature effects
Cochlear sensory epithelium and Corti organ degeneration after noise exposure in guinea pigs and cats, using scanning electron microscopy
Copper and gold films (0.2 to 2 microns) were ion plated onto polished 304-stainless-steel surfaces. These coatings were examined by scanning electron microscopy for coating growth defects. Three types of defects were distinguished: nodular growth, abnormal or runaway growth, and spits. The cause and origin for each type of defect was traced. Nodular growth is primarily due to inherent substrate microdefects, abnormal or runaway growth is due to external surface inclusions, and spits are due to nonuniform evaporation. All these defects have adverse effects on the coatings. They induce stresses and produce porosity in the coatings and thus weaken their mechanical properties. Friction and wear characteristics are affected by coating defects, since the large nodules are pulled out and additional wear debris is generated.
Geological samples are inherently multi-scale. Understanding their bulk physical and chemical properties requires characterization down to the nano-scale. A powerful technique to study the three-dimensional microstructure is X-ray tomography, but it lacks information about the chemistry of samples. To develop a methodology for measuring the multi-scale 3D microstructure of geological samples, correlative X-ray micro- and nanotomography were performed on two rocks followed by scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS) analysis. The study was performed in five steps: (i) micro X-ray tomography was performed on rock sample cores, (ii) samples for nanotomography were prepared using laser milling, (iii) nanotomography was performed on the milled sub-samples, (iv) samples were mounted and polished for SEM analysis and (v) SEM imaging and compositional mapping was performed on micro and nanotomography samples for complimentary information. Correlative study performed on samples of serpentine and basalt revealed multiscale 3D structures involving both solid mineral phases and pore networks. Significant differences in the volume fraction of pores and mineral phases were also observed dependent on the imaging spatial resolution employed. This highlights the necessity for the application of such a multiscale approach for the characterization of complex aggregates such as rocks. Information acquired from the chemical mapping of different phases was also helpful in segmentation of phases that did not exhibit significant contrast in X-ray imaging. Adoption of the protocol used in this study can be broadly applied to 3D imaging studies being performed at the Advanced Light Source and other user facilities.
Supplemental Data Files for a submission to Geosciences, "Using Fission-Track Radiography Coupled with Scanning Electron Microscopy for Efficient Identification of Solid-Phase Uranium Mineralogy at a Former Uranium Pilot Mill (Grand Junction, Colorado)"
Dental enamel, the outermost tissue of mammalian teeth, must withstand a lifetime of wear and cyclic contact. To meet this demand, enamel possesses a combination of high hardness and resistance to fracture, properties that are typically mutually exclusive. The impressive damage tolerance has been attributed largely to decussation of the enamel rods, the principal unit of its microstructure. As such, enamel is inspiring the design of next‐generation structural materials. However, quantitative descriptions of the decussated enamel rod microstructure remain limited due to challenges encountered in applying computed tomography and in acquiring quality images appropriate for traditional digital processing methods. Here, a machine learning segmentation method is applied to images of the enamel obtained using scanning electron microscopy to support quantitative analysis of the microstructure. A pretrained convolutional neural network is used to expand the input training image dataset to allow the training of a random forest classifier, which ultimately segments the image with a very small training set ( n = 3 images). A validation of this segmentation method is presented, in addition to its application to calculate relevant microstructural parameters for images of tooth enamel from selected mammalian species. The methodology applied here is equally applicable to other hard tissues.