Direct Detector Research Articles

Imaging built-in electric fields and light matter by Fourier-precession TEM

We report the precise measurement of electric fields in nanostructures, and high-contrast imaging of soft matter at ultralow electron doses by transmission electron microscopy (TEM). In particular, a versatile method based on the theorem of reciprocity is introduced to enable differential phase contrast imaging and ptychography in conventional, plane-wave illumination TEM. This is realised by a series of TEM images acquired under different tilts, thereby introducing the sampling rate in reciprocal space as a tuneable parameter, in contrast to momentum-resolved scanning techniques. First, the electric field of a p–n junction in GaAs is imaged. Second, low-dose, in-focus ptychographic and DPC characterisation of Kagome pores in weakly scattering covalent organic frameworks is demonstrated by using a precessing electron beam in combination with a direct electron detector. The approach offers utmost flexibility to record relevant spatial frequencies selectively, while acquisition times and dose requirements are significantly reduced compared to the 4D-STEM counterpart.

Measurements of dichroic bow-tie antenna arrays with integrated cold-electron bolometers using YBCO oscillators.

We consider properties of dichroic antenna arrays on a silicon substrate with integrated cold-electron bolometers to detect radiation at frequencies of 210 and 240 GHz. This frequency range is widely used in cosmic microwave background experiments in space, balloon, and ground-based missions such as BICEP Array, LSPE, LiteBIRD, QUBIC, Simons Observatory, and AliCPT. As a direct radiation detector, we use cold-electron bolometers, which have high sensitivity and a wide operating frequency range, as well as immunity to spurious cosmic rays. Their other advantages are the compact size of the order of a few micrometers and the effect of direct electron cooling, which can improve sensitivity in typical closed-loop cycle 3He cryostats for space applications. We study a novel concept of cold-electron bolometers with two SIN tunnel junctions and one SN contact. The amplitude-frequency characteristics measured with YBCO Josephson Junction oscillators show narrow peaks at 205 GHz for the 210 GHz array and at 225 GHz for the 240 GHz array; the separation of these two frequency bands is clearly visible. The noise equivalent power level at an operating point in the current bias mode is 5 × 10-16 W/√Hz.

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

Fast fabrication of μm-thick perovskite films by using a one-step doctor-blade coating method for direct X-ray detectors

The inclusion of a high-content crown ether in the perovskite precursor effectively increases the thickness of the doctor-bladed perovskite film and enhances the X-ray photoresponse of the direct X-ray detector.

Direct X-ray detectors made of zero-dimensional hybrid metal halide perovskite single crystals

A novel zero-dimensional cadmium hybrid metal halide (C19H18P)2CdCl4 single crystal was synthesized by inserting (C19H18P)+ into a [CdCl4]2− tetrahedron lattice through a slow volatilization method, which was proved to be a promising X-ray detector.

Atomic-level imaging of beam-sensitive COFs and MOFs by low-dose electron microscopy.

Electron microscopy, an important technique that allows for the precise determination of structural information with high spatiotemporal resolution, has become indispensable in unravelling the complex relationships between material structure and properties ranging from mesoscale morphology to atomic arrangement. However, beam-sensitive materials, particularly those comprising organic components such as metal-organic frameworks (MOFs) and covalent organic frameworks (COFs), would suffer catastrophic damage from the high energy electrons, hindering the determination of atomic structures. A low-dose approach has arisen as a possible solution to this problem based on the integration of advancements in several aspects: electron optical system, detector, image processing, and specimen preservation. This article summarizes the transmission electron microscopy characterization of MOFs and COFs, including local structures, host-guest interactions, and interfaces at the atomic level. Revolutions in advanced direct electron detectors, algorithms in image acquisition and processing, and emerging methodology for high quality low-dose imaging are also reviewed. Finally, perspectives on the future development of electron microscopy methodology with the support of computer science are presented.

Development of high-performance direct X-ray detector materials: from hybrid halide perovskites to all-inorganic lead-free perovskites

X-rays Detection plays a vital role in medical imaging, industrial defect detection, security screening and scientific research. Direct X-ray detectors are of greater interest to researchers because they offer the...

Sub 3Å cryoEM structure using a standard LaB6 120kV TEM upgraded with direct electron detector

Sub 3Å cryoEM structure using a standard LaB6 120kV TEM upgraded with direct electron detector

Recent Progress in Direct X-ray detectors Based on Metal Oxide Wide Bandgap Semiconductors: A Review

Recent Progress in Direct X-ray detectors Based on Metal Oxide Wide Bandgap Semiconductors: A Review

4D STEM in SEM with a Fast Pixelated Direct Detector

4D STEM in SEM with a Fast Pixelated Direct Detector

The Effect of Air Ionization in Testing Perovskite-Based Direct Conversion X-ray Detectors

The Effect of Air Ionization in Testing Perovskite-Based Direct Conversion X-ray Detectors

A simple, static and stage mounted direct electron detector based electron backscatter diffraction system

To engineer the next generation of advanced materials we must understand their microstructure, and this requires microstructural characterization. This can be achieved through the collection of high contrast, data rich, and insightful microstructural maps. Electron backscatter diffraction (EBSD) has emerged as a popular tool available within the scanning electron microscope (SEM), where maps are realized through the repeat capture and analysis of Kikuchi diffraction patterns. Typical commercial EBSD systems require large and sophisticated detectors that are mounted on the side of the SEM vacuum chamber which can be limiting in terms of widespread access to the technique. In this work, we present an alternative open-hardware solution based upon a compact EBSD system with a simple, static geometry that uses an off-the-shelf direct electron detector co-mounted with a sample. This simple stage is easy to manufacture and improves our knowledge of the diffraction geometry significantly. Microscope and detector control is achieved through software application programming interface (API) integration. After pattern capture, analysis of the diffraction patterns is performed using open-source analysis within AstroEBSD. To demonstrate the potential of this set up, we present two simple EBSD experiments using a line scan and area mapping. We hope that the present system can inspire simpler EBSD system design for widespread access to the EBSD technique and promote the use of open-source software and hardware in the workflow of EBSD experiments.

Generational assessment of EBSD detectors for cross-correlation-based analysis: From scintillators to direct detection

Introduced over ten years ago, cross-correlation-based electron backscatter diffraction has enabled high precision measurements of crystallographic rotations and elastic strain gradients at high spatial resolution. Since that time, there have been remarkable improvements in electron detector technology, including the advent of ultra-high speed detectors and the commercialization of direct detectors. In this study, we assess the efficacy of multiple generations of electron detectors for cross-correlation-based analysis using a single crystal Si sample as a reference. We show that, while improvements in precision are modest, there have been significant gains in the rate at which high-quality diffraction patterns can be collected. This has important implications in the size of datasets that can be collected and reduces the impact of drift and sample contamination.

Observation of Bacteriophage Ultrastructure by Cryo-Electron Microscopy.

Transmission electron microscopy (TEM) is an ideal method to observe and determine the structure of bacteriophages. From early studies by negative staining to the present atomic structure models derived from cryo-TEM, bacteriophage detection, classification, and structure determination have been mostly done by electron microscopy. Although embedding in metal salts has been a routine method for virus observation for many years, the preservation of bacteriophages in a thin layer of fast frozen buffer has proven to be the most convenient preparation method for obtaining images using cryo-electron microscopy (cryo-EM). In this technique, frozen samples are observed at liquid nitrogen temperature, and the images are acquired using different recording media. The incorporation of direct electron detectors has been a fundamental step in achieving atomic resolution images of a number of viruses. These projection images can be numerically combined using different approaches to render a three-dimensional model of the virus. For those viral components exhibiting any symmetry, averaging can nowadays achieve atomic structures in most cases. Image processing methods have also evolved to improve the resolution in asymmetric viral components or regions showing different types of symmetries (symmetry mismatch).

Deep Learning Approach for High-accuracy Electron Counting of Monolithic Active Pixel Sensor-type Direct Electron Detectors at Increased Electron Dose.

Electron counting can be performed algorithmically for monolithic active pixel sensor direct electron detectors to eliminate readout noise and Landau noise arising from the variability in the amount of deposited energy for each electron. Errors in existing counting algorithms include mistakenly counting a multielectron strike as a single electron event, and inaccurately locating the incident position of the electron due to lateral spread of deposited energy and dark noise. Here, we report a supervised deep learning (DL) approach based on Faster region-based convolutional neural network (R-CNN) to recognize single electron events at varying electron doses and voltages. The DL approach shows high accuracy according to the near-ideal modulation transfer function (MTF) and detector quantum efficiency for sparse images. It predicts, on average, 0.47 pixel deviation from the incident positions for 200 kV electrons versus 0.59 pixel using the conventional counting method. The DL approach also shows better robustness against coincidence loss as the electron dose increases, maintaining the MTF at half Nyquist frequency above 0.83 as the electron density increases to 0.06 e-/pixel. Thus, the DL model extends the advantages of counting analysis to higher dose rates than conventional methods.

Multi-exposure diffraction pattern fusion applied to enable wider-angle transmission Kikuchi diffraction with direct electron detectors

Diffraction pattern analysis can be used to reveal the crystalline structure of materials, and this information is used to nano- and micro-structure of advanced engineering materials that enable modern life. For nano-structured materials typically diffraction pattern analysis is performed in the transmission electron microscope (TEM) and TEM diffraction patterns typically have a limited angular range (less than a few degrees) due to the long camera length, and this requires analysis of multiple patterns to probe a unit cell. As a different approach, wide angle Kikuchi patterns can be captured using an on-axis detector in the scanning electron microscope (SEM) with a shorter camera length. These ‘transmission Kikuchi diffraction’ (TKD) patterns present a direct projection of the unit cell and can be routinely analysed using EBSD-based methods and dynamical diffraction theory. In the present work, we enhance this analysis significantly and present a multi-exposure diffraction pattern fusion method that increases the dynamic range of the detected patterns captured with a Timepix3-based direct electron detector (DED). This method uses an easy-to-apply exposure fusion routine to collect data and extend the dynamic range, as well as normalise the intensity distribution within these very wide (>95°) angle patterns. The potential of this method is demonstrated with full diffraction sphere reprojection and highlight potential of the approach to rapidly probe the structure of nano-structured materials in the scanning electron microscope.

Halide Perovskites and Their Derivatives for Efficient, High-Resolution Direct Radiation Detection: Design Strategies and Applications.

The past decade has witnessed a rapid rise in the performance of optoelectronic devices based on lead-halide perovskites (LHPs). The large mobility-lifetime products and defect tolerance of these materials, essential for optoelectronics, also make them well-suited for radiation detectors, especially given the heavy elements present, which is essential for strong X-ray and γ-ray attenuation. Over the past decade, LHP thick films, wafers, and single crystals have given rise to direct radiation detectors that have outperformed incumbent technologies in terms of sensitivity (reported values up to 3.5×106 µC Gyair -1 cm-2 ), limit of detection (directly measured values down to 1.5 nGyair s-1 ), along with competitive energy and imaging resolution at room temperature. At the same time, lead-free perovskite-inspired materials (e.g., methylammonium bismuth iodide), which have underperformed in solar cells, have recently matched and, in some areas (e.g., in polarization stability), surpassed the performance of LHP detectors. These advances open up opportunities to achieve devices for safer medical imaging, as well as more effective non-invasive analysis for security, nuclear safety, or product inspection applications. Herein, the principles behind the rapid rises in performance of LHP and perovskite-inspired material detectors, and how their properties and performance link with critical applications in non-invasive diagnostics are discussed. The key strategies to engineer the performance of these materials, and the important challenges to overcome to commercialize these new technologies are also discussed.

Focused ion beam milling and MicroED structure determination of metal-organic framework crystals

We report new advancements in the determination and high-resolution structural analysis of beam-sensitive metal organic frameworks (MOFs) using microcrystal electron diffraction (MicroED) coupled with focused ion beam milling at cryogenic temperatures (cryo-FIB). A microcrystal of the beam-sensitive MOF, ZIF-8, was ion-beam milled in a thin lamella approximately 150 nm thick. MicroED data were collected from this thin lamella using an energy filter and a direct electron detector operating in counting mode. Using this approach, we achieved a greatly improved resolution of 0.59 Å with a minimal total exposure of only 0.64 e−/A2. These innovations not only improve model statistics but also further demonstrate that ion-beam milling is compatible with beam-sensitive materials, augmenting the capabilities of electron diffraction in MOF research.

Time calibration studies for the Timepix3 hybrid pixel detector in electron microscopy

Direct electron detection is currently revolutionizing many fields of electron microscopy due to its lower noise, its reduced point-spread function, and its increased quantum efficiency. More specifically to this work, Timepix3 is a hybrid-pixel direct electron detector capable of outputting temporal information of individual hits in its pixel array. Its architecture results in a data-driven detector, also called event-based, in which individual hits trigger the data off the chip for readout as fast as possible. The presence of a pixel threshold value results in an almost readout-noise-free detector while also defining the hit time of arrival and the time the signal stays over the pixel threshold. In this work, we have performed various experiments to calibrate and correct the Timepix3 temporal information, specifically in the context of electron microscopy. These include the energy calibration, and the time-walk and pixel delay corrections, reaching an average temporal resolution throughout the entire pixel matrix of 1.37±0.04ns. Additionally, we have also studied cosmic rays tracks to characterize the charge dynamics along the volume of the sensor layer, allowing us to estimate the limits of the detector’s temporal response depending on different bias voltages, sensor thickness, and the electron beam ionization volume. We have estimated the uncertainty due to the ionization volume ranging from about 0.8 ns for 60 keV electrons to 8.8 ns for 300 keV electrons.

Optimization of visible photoluminescence emission from Ni-Zn ferrite thin films

Ni-Zn ferrite films with different thicknesses were prepared by the spray method, aiming to study the relationship between the annealing effect in an oxygen rich environment and the structural, optical properties and photoluminescence emission. X-ray diffraction (XRD) analysis used with Rietveld refinement showed that all prepared samples had a single spinel phase structure. Likewise, the Fourier transform infrared (FTIR) spectra confirmed the phase formation of Ni-Zn ferrites by appearing in both of the two characteristic absorption bands which are related to the tetrahedral and octahedral sites. For annealed thin film samples of Ni-Zn ferrite, the atomic force microscope (AFM) surface morphology exhibits pinning structure on the surface in nanoscale height, whereas for un-annealed samples, there are hills and valleys cover a broad region. The different electronic transitions were estimated from the UV-visible transmission spectrum. Strong photoluminescence (PL) intensity in the visible range was observed under the excitation of UV radiation. The intensity of the PL signal was strongest at a film thickness of 750 nm then decreased for higher thicknesses. This could be interpreted by using proposed energy level structures based on the transmission spectrum of the investigated samples. The strong PL intensity introduces the samples as a direct optical detector for UV radiation.