Electron Detector Research Articles

Direct method for microscale manipulation at liquid-liquid interfaces in ionic liquid media with real-time electron microscopy observation

A deep understanding of the processes in soft matter systems with liquid-liquid phase boundaries is of particular importance for materials science, chemistry and life sciences. A vast variety of physicochemical techniques have been proposed for the study of interfacial properties of liquid systems. Among them, electron microscopy methods occupy an important place due to the possibility of direct observation of the sample areas of interest with high spatial resolution; however, the harsh conditions of the electron microscope chamber impose significant restrictions on the possibilities of observing and manipulating unprotected liquids and related soft systems. To overcome these difficulties, in this work, we developed a methodology for direct probing of liquid-liquid interfaces with simultaneous control of the process using electron microscopy. Practically relevant liquid mixtures based on vacuum-compatible ionic liquid (IL) with water additives were probed with micrometer accuracy in real time inside an electron microscope chamber, which made it possible to reveal the role of specific ions aggregation and electrostatic phenomena in the stabilization of liquid microdomains. To test the versatility of the proposed approach, the morphology of a typical IL/water mixture was examined using a series of electron microscopes of various configurations, and it was shown that the best level of contrast between two chemically related liquid phases can be obtained in the case of a cold field emission electron source in combination with an in-lens secondary electron detector, regardless of the specific instrument manufacturer.

Acceptance characterization of electron detector in SEM using stainless steel sphere.

Although modern scanning electron microscope (SEM) possess several electron detectors, it is not clear what kind of information is contained in a SEM image taken by a certain detector. Especially the detectors installed in the objective lens are difficult to know their characters. Thus, we propose a simple method to assess the acceptance of electron detector using a stainless-steel sphere. After taking images under certain conditions, say electron beam energy, working distance etc., the image intensity of each pixel point, which is characterized by coordinate (θ, φ), is evaluated. The advantage of this method is the ease of implementation and the whole information of electron emission from the tilted surfaces is contained in the image. Using this information, the acceptance of the detector can be analyzed systematically. In this paper, the traditional Everhart-Thornley detector is analyzed with this method. It is demonstrated how the sphere image changes according to the measurement condition. The ET image quality is strongly governed by working distance but not so much by the electron beam energy. We propose an alternative method to avoid the ambiguity of working distance. Using a needle type specimen stage, the ET image does not vary so much with WD and the reliability of ET image significantly improves.

The investigation of endodontic irrigants and polyhexanide-based solution action on smear layer

AIM. The effect of irrigants on the smear layer on the intracanalicular dentin surface is one of the important issues in endodontics. The objective of this article is to determine the effect of different concentrations of polyhexanide-based solutions and standard irrigants on the smear layer using scanning electron microscopy (SEM).MATERIALS AND METHODS. The present study was conducted on 42 extracted teeth (third molars, first and second premolars) with formed apices that had been extracted for orthodontic indications. The teeth were decoronated and samples were prepared. In order to create a smear layer, the lumen of the canals was instrumented with H-file #40 throughout. A simulation of root canal irrigation was conducted by immersing the specimens in a 5-ml container filled with the proper solution for 1 hour: group 1 – no treatment (n = 6); group 2 – saline (n = 6); group 3 – 2% chlorhexidine (n = 6); group 4 – 3% sodium hypochlorite (n = 6); group 5 – 17% EDTA; group 6 – polyhexanide 0.1% (n = 6); group 7 – polyhexanide 0.2% (n = 6). A ~30 nm thick platinum film was sputtered onto the surface of each sample using a magnetron deposition technique. SEM microphotos were acquired on a Vega3 TESCAN scanning electron microscope (SEM) with an SE secondary electron detector, which enables imaging with high topographic contrast. The initial detector (incamera) was employed for image acquisition, with an electron energy of 30 keV. Images were acquired at magnifications of x20 (overview image), x150, x250, x500, x1000, x2500, x7500 for each sample.RESULTS. The samples from groups 1 and 5 demonstrated the absence of a smear layer on the dentin surface and the absence of smear plugs in the dentinal tubules. Groups 2 and 3 are distinguished by the deposition of a pronounced amorphous smear layer and the obturation of all dentinal tubules. Groups 4, 6, and 7 are distinguished by the deposition of a smaller volume of smear layer on the dentin surface, as well as the presence of semi-open or completely open entrances to the dentinal tubules.CONCLUSION. The data obtained indicates that antiseptic compositions based on polyhexanide in concentrations of 0.1 and 0.2% do not have a pronounced effect on the smear layer. However, in visual evaluation of SEM micrographs, their effect is comparable to that of 3% sodium hypochlorite. In instances where enhanced dissolution of the smear layer and smear plugs from the tubules is necessary to facilitate decontamination of the wall dentin, the combination of antiseptics with chelate compounds, such as 17% EDTA, may be employed.

Near-Infrared Polarization-Sensitive Detection by All-Si Plasmonic Hot Electron Detectors.

Polarization-sensitive optoelectronic detection has been achieved by an all-Si detector in the NIR range, based on plasmon hot electron generation/internal photoemission effect. An advanced architecture with a specially designed anisotropic metasurface was developed and structurally optimized for maximizing the internal quantum efficiency (IQE). Assisted by finite difference time domain (FDTD) simulations, the well-designed device exhibits a maximum optical absorption of 80% around 1.45 μm, corresponding to an optical discrimination ratio of 120. Optoelectronic measurements show the peak responsivity and detectivity of 51.2 mA/W and 8.05 × 1010 cm Hz1/2/W, respectively, at 1.45 μm. A high polarization photocurrent ratio of 35 nm is also achieved at 1.55 μm. Moreover, the optoelectronic response can be tuned by a back-gate bias. Last but not least, we built up a model for theoretically estimating the IQE, which provides instructive guidance for further enhancing the optoelectronic performance of hot electron detectors.

Large-Angle Rocking Beam Electron Diffraction of Large Unit Cell Crystals Using Direct Electron Detector.

We report a large-angle rocking beam electron diffraction (LARBED) technique for electron diffraction analysis. Diffraction patterns are recorded in a scanning transmission electron microscope (STEM) using a direct electron detector with large dynamical range and fast readout. We use a nanobeam for diffraction and perform the beam double rocking by synchronizing the detector with the STEM scan coils for the recording. Using this approach, large-angle convergent beam electron diffraction (LACBED) patterns of different reflections are obtained simultaneously. By using a nanobeam, instead of a focused beam, the LARBED technique can be applied to beam-sensitive crystals as well as crystals with large unit cells. This paper describes the implementation of LARBED and evaluates the performance using silicon and gadolinium gallium garnet crystals as test samples. We demonstrate that our method provides an effective and robust way for recording LARBED patterns and paves the way for quantitative electron diffraction of large unit cell and beam-sensitive crystals.

Application of Optical-electron Correlative Microscopy for Characterization of Organic Matter

ABSTRACT Application of coal petrology is known to play significant role in several industrial sectors viz. thermal industries, steel industries, unconventional oil and gas fields. One important aspect of organic matter characterization, especially for unconventional oil and gas fields is the development of organic matter hosted porosity, and commonly Scanning Electron Microscopy (SEM) is used to study the same. While, SEM helps in understanding the nature of porosity developed in coals and shales, one significant limitation is that under SEM the different organic matter types can’t be distinguished, as all organic matter appears dark due to their lower atomic mass. Optical-electron correlative microscopy has recently gained importance for making advancement in addressing the abovementioned scientific gap. While this method has been found some usage for characterizing the dispersed organic matter in shales, only one work globally exists where the technique has been used for studying coals. In this work, possibly, for the first time, this technique is applied for characterizing three Indian coals from Korba basin, India, with the main objective of establishing necessary protocols for reliable imaging of different organic matter types under SEM. Our results establish that imaging under SEM using Backscattered electron (BSE) detector, the macerals and mineral matter were clearly discernible at 15 kV accelerating voltage. Further, this exercise also indicates that identification of vitrinite macerals under SEM, without correlative technique can be challenging, while some inertinites with their distinctive structures can be identified under stand-alone SEM. Sporinites too, due to their distinctive morphology, were easily identifiable under SEM.

Development of electron detectors for the BRAND experiment

The BRAND experiment employs detectors that utilize gas ionization and plastic scintillators, integrated with custom-designed front-end electronics, aimed at measuring the correlation coefficients in neutron beta decay. This article focuses on the characterization and performance of a newly developed electron detector prototype featuring custom-designed front-end electronics. The characterization results indicate an weak gain dependency of the scintillator when exposed to a radioactive source, varying along its length and width.

On the temporal transfer function in STEM imaging from finite detector response time

Faster scanning in scanning transmission electron microscopy has long been desired for the ability to better control dose, minimise effects of environmental distortions, and to capture the dynamics of in-situ experiments. Advances in scan controllers and scan deflection systems have enabled scanning with pixel dwell times on the order of tens of nanoseconds. At these speeds, the finite response time of the electron detector must be considered as the signal from one electron detection event can contribute to multiple pixels, blurring the features within the image. Here we introduce a temporal transfer function (TTF) to describe and model the effects of detector response time on imaging, as well as a framework for incorporating these effects into simulation.

Coherent long-term average indoor radon concentration estimates obtained by electronic and solid state nuclear track detectors

Despite the rapid development of consumer-grade electronic radon monitors, their capabilities to assess long-term average radon concentrations are not systematically investigated. We present the results of a year-long measurement campaign in 32 dwellings and workplaces in two areas with typical and high radon concentrations in Bulgaria. A systematic comparison was made between electronic monitors and the gold standard — solid-state nuclear track detectors (SSNTDs). RadonEye Plus2 (RE) monitors were used, calibrated and metrologically tested at the three participating laboratories. Two SSNTD-based detectors were utilized: passive radon detectors (PRDs) developed by UKHSA, and CDs/DVDs, developed at SU. Two PRDs for quarterly radon measurements, a RE, a CD and a DVD were placed at each location. Additional old CDs/DVDs were collected for retrospective radon estimates. The results for the annual average radon concentrations, estimated by the four methods are presented. The average difference between the REs and PRDs estimate was 8% (median 4%), between the REs and CDs was 5% (median 0.4%) and between REs and DVDs was −10% (median −12%). The Z-score, representing the difference normalized to its uncertainty, in most cases fell within −1 and 1, indicating excellent agreement. The retrospective estimates also demonstrated excellent agreement with the other data. However, in some cases, small but statistically significant biases were identified between REs and SSNTDs or between different SSNTDs, requiring an inclusion of a reference instrument in future studies. Overall, the results imply that with sound metrological assurance, RadonEye Plus2 monitors can assess long-term average radon concentrations with sufficient accuracy.

First observation results of Macao Science Satellite 1 on lightning-induced electron precipitation

AbstractThe mid-energy electron detector (MEED) is a space-borne instrument onboard Macao Science Satellite 1 (MSS-1) dedicated to monitoring the typical charged particle radiation characteristics in the satellite orbit and the process of their occurrence and development, including short bursts of lightning-induced electron precipitation (LEP). This paper presents the first results of the LEP measurements by the MSS-1. 47 LEP events are identified with the routine operation for 3 months since satellite launch, all within the range of 1.5<L<3.0 (where L represents the McIlwain L-parameter), and the causative lightning discharges are definitively geo-located for these LEP events. The LEP events occur within <1 s of the causative lightning and consist of 40–300 keV electrons. A preliminary observation result indicates that, with medium-energy electron detectors, MSS-1 can present in-situ observations of large regions of enhanced background precipitation and reveal their fine spatiotemporal characteristics and spectral signatures. The collaborative VLF ground-based measurements at the Great Wall Station, Antarctica also have a good correspondence with LEP measurements of MSS-1. The observations also imply that lightning activity has a modulation effect on the energetic electron energy-spatial structure.

Linear response theory for light dark matter-electron scattering in materials

We combine the nonrelativistic effective theory of dark matter (DM)-electron interactions with linear response theory to obtain a formalism that fully accounts for screening and collective excitations in DM-induced electronic transition rate calculations for general DM-electron interactions. In the same way that the response of a dielectric material to an external electric field in electrodynamics is described by the dielectric function, so in our formalism the response of a detector material to a DM perturbation is described by a set of which can be directly related to densities and currents arising from the nonrelativistic expansion of the Dirac Hamiltonian. We apply our formalism to assess the sensitivity of non-spin-polarized detectors, and find that in-medium effects significantly affect the experimental sensitivity if DM couples to the detector's electron density, while being decoupled from other densities and currents. Our formalism can be straightforwardly extended to the case of spin-polarized materials. Published by the American Physical Society 2024

Energy filtering enables macromolecular MicroED data at sub-atomic resolution.

High resolution information is important for accurate structure modelling. However, this level of detail is typically difficult to attain in macromolecular crystallography because the diffracted intensities rapidly fade with increasing resolution. The problem cannot be circumvented by increasing the fluence as this leads to detrimental radiation damage. Previously, we demonstrated that high quality MicroED data can be obtained at low flux conditions using electron counting with direct electron detectors. The improved sensitivity and accuracy of these detectors essentially eliminate the read-out noise, such that the measurement of faint high-resolution reflections is limited by other sources of noise. Inelastic scattering is a major contributor of such noise, increasing background counts and broadening diffraction spots. Here, we demonstrate that a substantial improvement in signal-to-noise ratio can be achieved using an energy filter to largely remove the inelastically scattered electrons. This strategy resulted in sub-atomic resolution MicroED data from proteinase K crystals, enabling accurate structure modelling and the visualization of detailed features. Interestingly, filtering out the noise revealed diffuse scattering phenomena that can hold additional structural information. Our findings suggest that combining energy filtering and electron counting can provide more accurate measurements at higher resolution, providing better insights into protein function and facilitating more precise model refinement.

A multi-satellite survey scheme for addressing open questions on the Earth’s outer radiation belt dynamics

The Earth’s outer radiation belt is highly dynamic, containing relativistic electron fluxes that can increase by several orders of magnitude during magnetospheric disturbances. This greatly increases the likelihood of spacecraft malfunction or failure and significantly influences the solar-terrestrial system’s energy and mass coupling, highlighting the importance of fully understanding the mechanisms governing these dynamics from both theoretical and practical perspectives. Although many theories have been proposed, further research is essential to quantify the specific contributions of different dynamic mechanisms for improving space weather forecasting. To address this, observations of the outer radiation belt with high spatial–temporal resolution to distinguish the spatial and temporal variations are essential. We introduce a 10-CubeSat constellation survey scheme in the geosynchronous transfer orbit (GTO) to achieve this required observation. Three baseline instruments are proposed to be employed: the high energy electron detector (HEED), the search coil wave detector (SCWD), and the magnetometer (MAG). Two groups of physical processes will be investigated: wave-particle interactions involving charged particles interacting with whistler-mode waves, electromagnetic ion cyclotron (EMIC) waves, and ultra-low frequency (ULF) waves; and radial transport encompassing shock-induced injections, substorm injections, storm convection and magnetopause shadowing. The performance parameters of instruments and platform of the constellation are presented. Additionally, aligned with the concept of constellation survey, we outline the COSPAR-coordinated space program, COnstellation of Radiation BElt Survey (CORBES), which will provide a crucial scientific contribution in the absence of the Van Allen Probes. The program’s excellent observational capability enables a comprehensive understanding of the underlying physical mechanisms governing the outer radiation belt dynamics and improved space weather forecasting.

Improved Phase Discrimination in Power Plant Steels using In-Column Secondary Electron Detectors and Spherical Indexing

Improved Phase Discrimination in Power Plant Steels using In-Column Secondary Electron Detectors and Spherical Indexing

The Importance of an Open Camera System Demonstrated with Wide-ranging Applications of MerlinEM, Hybrid Pixel Direct Electron Detector for Scanning Transmission Electron Microscopy

The Importance of an Open Camera System Demonstrated with Wide-ranging Applications of MerlinEM, Hybrid Pixel Direct Electron Detector for Scanning Transmission Electron Microscopy

An Advanced Smart Counting Mode for Pixelated Direct Electron Detectors Based on Semiconductors

An Advanced Smart Counting Mode for Pixelated Direct Electron Detectors Based on Semiconductors

In Situ Study of the Activation Process of MOF-74 Using Three-Dimensional Electron Diffraction.

Metal-organic framework (MOF)-74 is known for its effectiveness in selectively capturing carbon dioxide (CO2). Especially the Zn and Cu versions of MOF-74 show high efficiency of this material for CO2. However, the activation of this MOF, which is a crucial step for its utilization, is so far not well understood. Here, we are closing the knowledge gap by examining the activation using, for the first time in the MOF, three-dimensional electron diffraction (3DED) during in situ heating. The use of state-of-the-art direct electron detectors enables rapid acquisition and minimal exposure times, therefore minimizing beam damage to the very electron beam-sensitive MOF material. The activation process of Zn-MOF-74 and Cu-MOF-74 is systematically studied in situ, proving the creation of open metal sites. Differences in thermal stability between Zn-MOF-74 and Cu-MOF-74 are attributed to the strength of the metal-oxygen bonds and Jahn-Teller distortions. In the case of Zn-MOF-74, we observe previously unknown remaining electrostatic potentials inside the MOF pores, which indicate the presence of remaining atoms that might impede gas flow throughout the structure when using the MOF for absorption purposes. We believe our study exemplifies the significance of employing advanced characterization techniques to enhance our material understanding, which is a crucial step for unlocking the full potential of MOFs in various applications.

Using Mössbauer Spectroscopy to Evaluate the Influence of Heat Treatment on the Surface Characteristics of Additive Manufactured 316L Stainless Steel.

The oxidation behaviour of iron-based 316L stainless steel was investigated in the temperature range of 700 to 1000 °C. The test specimens in the shape of plates were produced by selective laser melting. After fabrication, the samples were sandblasted and then annealed in air for different periods of time (0.5, 2, 8, 32 h). Under the influence of temperature and time, stainless steels tend to form an oxide layer. Scanning electron microscopy, energy dispersive analysis, and X-ray diffraction were employed to analyse the composition of this layer. Notably, a thin oxide layer primarily composed of (Fe-Cr) formed on the surface due to temperature effects. In addition, with increasing temperature (up to 1000 °C), the oxide of the main alloying elements, specifically Mn2(Fe-Cr)O4, appeared alongside the Fe-Cr oxide. Furthermore, the samples were subjected to conversion X-ray (CXMS) and conversion electron (CEMS) Mössbauer spectroscopy. CXMS revealed a singlet with a decreasing Mössbauer effect based on the surface metal oxide thickness. CEMS revealed the presence of Fe3+ in the surface layer (0.3 µm). Moreover, an interesting phenomenon occurred at higher temperature levels due to the inhomogeneously thick surface metal oxide layer and the tangential direction of the Mössbauer radiation towards the electron detector.

The Capture of Cadmium from Solution during the Replacement of Calcite by Apatite.

The capture of cadmium (Cd) from phosphate-containing solutions during the replacement of CaCO3 by phosphate phases such as hydroxylapatite (HAP) and tricalcium phosphate (TCP) has been studied under high and low temperature and pressure conditions using atomic force microscopy, scanning electron microscopy equipped with an X-ray spectrometer and a backscattered electron detector, Raman spectroscopy, and microprobe analysis. Starting with cubes of Carrara Marble (polycrystalline calcite) and single crystals of calcite, a new solid phosphate phase was observed to incorporate Cd from solution, formed under different pressure and temperature conditions tested. Results showed that Cd precipitated in a new phase on the surface of all samples tested. In Carrara Marble, pseudomorphic replacement of CaCO3 is restricted possibly due to kinetic limitation caused by the adsorption of Cd complexes formed in solution at reactive surface sites and the variation of fluid composition inside the sample. However, on the sample surface, this kinetic limitation is less influential, so the new phase could incorporate higher amounts of Cd faster. Furthermore, this reaction at room temperature was found to have similar and/or better Cd-uptake efficiency as HAP and CaCO3 in pure Cd solution through the precipitation of Cd-containing phosphate crystals on the sample surface. Both reactions were able to capture Cd in the precipitating phase structure and could provide a mechanism for simultaneous Cd and phosphate removal from solutions contaminated with both, in industrial or natural settings.

Reconstruction of 400 GeV/c proton interactions with the SHiP-charm project

The SHiP-charm project was proposed to measure the associated charm production induced by 400 GeV/c protons in a thick target, including the contribution from cascade production. An optimisation run was performed in July 2018 at CERN SPS using a hybrid setup. The high resolution of nuclear emulsions acting as vertex detector was complemented by electronic detectors for kinematic measurements and muon identification. Here we present first results on the analysis of nuclear emulsions exposed in the 2018 run, which prove the capability of reconstructing proton interaction vertices in a harsh environment, where the signal is largely dominated by secondary particles produced in hadronic and electromagnetic showers within the lead target.