Energy Filtering Research Articles

Electronic structure of partially fluorinated graphene: The impact of adsorption patterns and dynamic stability

The impact of fluorination on the stability and electronic structure of graphene is investigated by employing density functional theory calculations. It is observed that both the cell symmetry and dynamical stability (phonon dispersion spectra) are necessary for the identification of energetically optimum configurations. In general, an increase in band gap is observed with fluorination, which is in good agreement with the experimental studies. These results underscore the importance of employing key stability (energy, dynamical and thermal) filters for correct assessment of electronic properties of partially fluorinated graphene and may help to explain the inconsistencies of previous theoretical and experimental findings.

Elastic and inelastic mean free paths for scattering of fast electrons in thin-film oxides

Quantitative transmission electron microscopy (TEM) often requires accurate knowledge of sample thickness for determining defect density, structure factors, sample dimensions, electron beam and X-ray photons signal broadening. The most common thickness measurement is by Electron Energy Loss Spectroscopy which can be applied effectively to crystalline and amorphous materials. The drawback is that sample thickness is measured in units of Inelastic Mean Free Path (MFP) which depends on the material, the electron energy and the collection angle of the spectrometer.Furthermore, the Elastic MFP is an essential parameter for selecting optimal sample thickness to reduce dynamical scatterings, such as for short-range-order characterization of amorphous materials.Finally, the Inelastic to Elastic MFP ratio can predict the dominant mechanism for radiation damage due to the electron beam.We implement a fast and precise method for the extraction of inelastic and elastic MFP values in technologically important oxide thin films. The method relies on the crystalline Si substrate for calibration. The Inelastic MFP of Si was measured as a function of collection semi-angle (β) by combining Energy-Filtered TEM thickness maps followed by perpendicular cross-sectioning of the sample by Focused-Ion-Beam. For example, we measured a total Inelastic MFP (β∼157 mrad) in Si of 145 ± 10 nm for 200 keV electrons.The MFP of the thin oxide films is determined by their ratio at their interface with Si or SiO2. The validity of this method was verified by direct TEM observation of cross-to-cross sectioning of TEM samples. The high precision of this method was enabled mainly by implementing a wedge preparation technique, which provides large sampling areas with uniform thickness.We measured the Elastic and Inelastic Mean Free Paths for 200 keV and 80 keV electrons as a function of collection angle for: SiO2 (Thermal, CVD), low-κ SiOCH, Al2O3, TiO2, ZnO, Ta2O5 and HfO2.The measured MFP values were compared to calculations based on models of Wenzel, Malis and Iakoubovskii. These models deviate from measurements by up to 30%, especially for 80 keV electrons. Hence, we propose functional relations for the Elastic MFP and Inelastic MFP in oxides with respect to the mass density and effective atomic number, which reduce deviations by a factor of 2–3. In addition, the effects of sample cooling on the measurements and sample stability are examined.

Optical-Beam-Induced Current in InAs/InP Nanowires for Hot-Carrier Photovoltaics.

Using the excess energy of charge carriers excited above the band edge (hot carriers) could pave the way for optoelectronic devices, such as photovoltaics exceeding the Shockley–Queisser limit or ultrafast photodetectors. Semiconducting nanowires show promise as a platform for hot-carrier extraction. Proof of principle photovoltaic devices have already been realized based on InAs nanowires, using epitaxially defined InP segments as energy filters that selectively transmit hot electrons. However, it is not yet fully understood how charge-carrier separation, relaxation, and recombination depend on device design and on the location of optical excitation. Here, we introduce the use of an optical-beam-induced current (OBIC) characterization method, employing a laser beam focused close to the diffraction limit and a high precision piezo stage, to study the optoelectric performance of the nanowire device as a function of the position of excitation. The photocurrent response agrees well with modeling based on hot-electron extraction across the InP segment via diffusion. We demonstrate that the device is capable of producing power and estimate the spatial region within which significant hot-electron extraction can take place to be on the order of 300 nm away from the barrier. When comparing to other experiments on similar nanowires, we find good qualitative agreement, confirming the interpretation of the device function, while the extracted diffusion length of hot electrons varies. Careful control of the excitation and device parameters will be important to reach the potentially high device performance theoretically available in these systems.

Improving electrical and thermal properties synchronously via introducing CsPbBr3 QDs into higher manganese silicides

Higher manganese silicide (HMS) is a P-type medium temperature thermoelectric (TE) material, which has attracted widespread attention over the past few decades due to its remarkable mechanical properties, excellent chemical and thermal stability, as well as the non-toxicity, abundance and competitive price. The peak power factor (PF) of HMS is as high as ∼1.50 × 10−3 W m−1 K−2 because of its intrinsic high electrical conductivity and Seebeck coefficient. However, the thermal conductivity of HMS is also high, resulting in relatively low zT values. Introducing nano-dispersion in the matrix is one of the most effective methods to enhance the TE properties via reducing the lattice thermal conductivity significantly without drastic changes on the other parameters. In this study, CsPbBr3 QDs with uniform size were synthesized and introduced into HMS bulks. The PF (at 823 K) was enhanced to 1.71 × 10−3 W m−1 K−2, which is improved 14.0% approximately compared with that of pure HMS owing to the combined effect of element doping and energy filtering. The lattice thermal conductivity (at 823 K) decreased from 2.56 W m−1 K−1 to 1.99 W m−1 K−1 synchronously (∼22.0%) due to the intensive phonon scattering caused by Cs doping, and the embedding of Pb riched CsPbBr3 QDs and Pb QDs. A maximum zT value of 0.57 (823 K) is achieved in CsPbBr3 QDs/HMS composites, which is 36.0% higher than that of pure HMS. Predictably, for other TE materials, it is also feasible to improve the TE properties via introducing metastable quantum dots.

TREPs-A New Class of Functional tRNA-Encoded Peptides.

We asked if transfer RNA (tRNA) ever got an opportunity of translating its own sequence during evolution, what would have been the function of such tRNA-encoded peptides (tREPs)? If not, could one artificially synthesize tREPs to study the corresponding functional outcomes? Here, we report a novel, first-in-the-class, chemically synthesized tREP-18 molecule originating from the Escherichia coli tRNA sequence showing potent antileishmanial property. As a first step, E. coli tRNAs were computationally translated into peptide sequence equivalents and a database of full-length hypothetical tREPs was created. The tREP sequences were sent into sequence, structure, and energy filters to narrow down potential peptides for experimental validation. Based on the functional predictions, tREPs were screened against antiparasitic targets, leading to the identification of tREP-18 as a potential antiparasitic peptide. The in vitro assay of chemically synthesized tREP-18 on the Ag83 strain of Leishmania donovani showed its potent antileishmanial property (IC50 value of 22.13 nM). The atomic force microscopy and scanning electron microscopy images indicated significant alteration in the cytoskeletal architecture of tREP-18-treated parasites. Also, tREP-18 seems to destabilize the mitochondrial membrane potential of parasites, disrupting their cellular integrity and leading to parasitic death. The cellular assays of the tREP-18 peptide on the BS12 strain, a clinical isolate of post-kala azar dermal leishmaniasis, demonstrated its significant efficacy at an IC50 value of 15 nM. The tREP-18 peptide showed a toxic effect on the amastigote stage of the parasite, showing macrophage pathogen clearance at a concentration of 22.5 nM. This study provides the proof of the concept of making a new class of functional peptides from tRNA sequences. It also opens a huge untapped tRNA-peptide space toward novel discoveries and applications. In the future, it would be interesting to perform tREP edits and redesign tREPs toward specific applications.

Quantitative composition determination by ADF-STEM at a low-angular regime: a combination of EFSTEM and 4DSTEM

High-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) is a valuable method for composition determination of nanomaterials. However, light elements do not scatter efficiently into the scattering angles employed for HAADF-STEM which hinders the composition determination of material systems containing light elements by HAADF-STEM. This makes the usage of lower scattering angles favourable. Moreover, static atomic displacements (SADs) caused by the small covalent radius of the substituting light elements in semiconductor alloys increase the scattering intensity at low angles. Nevertheless, at low angles, a quantitative match between complementary image simulations and experiments is not straight forward, since e.g. inelastic scattering and correlated phonon movement is often neglected in simulations.In this study, we establish a method to quantify material systems containing light elements at low angles by resolving the remaining sources of discrepancy. An outstanding agreement between simulations and experiments is achieved by using a combination of an in-column energy filter and a fast pixelated detector. By applying this method to GaNxAs1-x quantum wells, a good agreement of the TEM results with results from high-resolution x-ray diffraction is obtained. The method developed enables the nanoscale analysis of functional materials containing light elements, especially in the presence of SADs.

Serrated flow in nickel base super alloy 720Li at 350 and 450 °C: Effect of chromium and cobalt segregation at dislocation core

The tensile flow behavior of nickel base super alloy 720Li is investigated in the temperature range of 25 to 720 °C. At 350 and 450 °C, 720Li alloy exhibits serrated flow and the cause for the same is solute segregation at the dislocation core. From the energy filter transmission electron microscopy (EF-TEM) examination, it is evident that chromium segregation at dislocation core at 350 °C and chromium and cobalt segregation at dislocation core at 450 °C are primarily responsible for serrated flow in 720Li alloy.

Optimization of energy production in two-qubit heat engines using the ecological function

We study the ecological regime of quantum heat engines where the heat transfer between the environment and the engine is mediated with two qubits that act as energy filters and allow the conversion of heat into work. Using quantum thermodynamics, the theory of open quantum system and the fundamentals of finite-time thermodynamics we obtain the output power, the ecological function and the entropy production of the engine. Then, we optimize the functioning to the ecological function to find the range of efficiencies for which the system works optimally under the ecological criterium. We find that (i) the maximum value of the ecological function depends on the thermal copulings and the energies of the qubits that define the engine. (ii) We can define an ecological working region where the engine works producing a power that is similar to the maximum power but where it rejects much less heat to the environment. (iii) That the range of efficiencies defining the ecological region depends on the parameters defining the engine.(iv) An optimal working region where both the power and the ecological function are big is defined for each machine.

Enhancing Efficiency of Nonfullerene Organic Solar Cells via Using Polyelectrolyte-Coated Plasmonic Gold Nanorods as Rear Interfacial Modifiers.

Sufficient sunlight absorption and exciton generation are critical for developing efficient nonfullerene organic solar cells (OSCs). In this work, polyelectrolyte polystyrenesulfonate (PSS)-coated plasmonic gold nanorods (GNRs@PSS) were incorporated, for the first time, into the inverted nonfullerene OSCs as rear interfacial modifiers to improve sunlight absorption and charge generation via the near-field plasmonic and backscattering effects. The plasmonic GNRs effectively improved the sunlight absorption and enhanced the charge generation. Meanwhile, the negatively charged PSS shell ensured the uniform dispersion of the GNRs on the surface of the photoactive layer, optimized the interfacial contact, and further promoted the hole transport to the electrode. These concerted synergistic effects augmented the efficiency (10.11%) by nearly 20% relative to the control device (8.47%). Remarkably, the ultrathin (∼2.2 nm) organic layer on the surface of GNRs was closely examined by acquiring the carbon contrast image through energy-filtered transmission electron microscopy (EF-TEM), which clearly confirmed the coating uniformity from the side to end-cap of GNRs. The surface plasmon resonance (SPR) effect of the GNRs@PSS on the surface of the photoactive layer was unprecedentedly mapped by photoinduced force microscopy (PiFM) under the illumination of a tunable wavelength supercontinuum laser mimicking sunlight. Furthermore, investigations into the effect of size, surface coverage, and incorporation location of GNRs@PSS on the performance of OSCs revealed that the appropriate design and incorporation of the plasmonic nanostructures are crucial, otherwise the performance can be decreased, as evidenced in the case of front interface integration.

High-Energy Electron Scattering in Thick Samples Evaluated by Bright-Field Transmission Electron Microscopy, Energy-Filtering Transmission Electron Microscopy, and Electron Tomography.

Energy-filtering transmission electron microscopy (TEM) and bright-field TEM can be used to extract local sample thickness $t$ and to generate two-dimensional sample thickness maps. Electron tomography can be used to accurately verify the local $t$. The relations of log-ratio of zero-loss filtered energy-filtering TEM beam intensity ($I_{{\rm ZLP}}$) and unfiltered beam intensity ($I_{\rm u}$) versus sample thickness $t$ were measured for five values of collection angle in a microscope equipped with an energy filter. Furthermore, log-ratio of the incident (primary) beam intensity ($I_{\rm p}$) and the transmitted beam $I_{{\rm tr}}$ versus $t$ in bright-field TEM was measured utilizing a camera before the energy filter. The measurements were performed on a multilayer sample containing eight materials and thickness $t$ up to 800 nm. Local thickness $t$ was verified by electron tomography. The following results are reported:•The maximum thickness $t_{{\rm max}}$ yielding a linear relation of log-ratio, $\ln ( {I_{\rm u}}/{I_{{\rm ZLP}}})$ and $\ln ( {I_{\rm p}}/{I_{{\rm tr}}} )$, versus $t$.•Inelastic mean free path ($\lambda _{{\rm in}}$) for five values of collection angle.•Total mean free path ($\lambda _{{\rm total}}$) of electrons excluded by an angle-limiting aperture.•$\lambda _{{\rm in}}$ and $\lambda _{{\rm total}}$ are evaluated for the eight materials with atomic number from $\approx$10 to 79.The results can be utilized as a guide for upper limit of $t$ evaluation in energy-filtering TEM and bright-field TEM and for optimizing electron tomography experiments.

The optimum configuration design of a nanostructured thermoelectric device with resonance tunneling

A nanostructured thermoelectric device is designed by connecting a double-barrier resonant tunneling heterostructure to two electron reservoirs. Based on Landauer’s equation and Fermi–Dirac statistics, the exact solution of the heat flow is calculated. The maximum power output and efficiency are calculated through the optimizations of several key parameters. The optimum characteristic curve of the performance is obtained. The thermodynamic performance characteristics of thermodynamic device are analyzed, including output power and efficiency, and the optimal operation region of device is determined by optimize the main parameter. The results obtained show that the heterojunction may become a perfect energy filter by appropriately regulating the chemical potentials of electron reservoirs and optimally choosing the widths of barrier and quantum well and the nanostructured thermoelectric device with resonance tunneling may obtain simultaneously a large power output and a high efficiency.

Exploring high-resolution cryo-ET and subtomogram averaging capabilities of contemporary DEDs

The potential of energy filtering and direct electron detection for cryo-electron microscopy (cryo-EM) has been well documented. Here, we assess the performance of recently introduced hardware for cryo-electron tomography (cryo-ET) and subtomogram averaging (STA), an increasingly popular structural determination method for complex 3D specimens. We acquired cryo-ET datasets of EIAV virus-like particles (VLPs) on two contemporary cryo-EM systems equipped with different energy filters and direct electron detectors (DED), specifically a Krios G4, equipped with a cold field emission gun (CFEG), Thermo Fisher Scientific Selectris X energy filter, and a Falcon 4 DED; and a Krios G3i, with a Schottky field emission gun (XFEG), a Gatan Bioquantum energy filter, and a K3 DED. We performed constrained cross-correlation-based STA on equally sized datasets acquired on the respective systems. The resulting EIAV CA hexamer reconstructions show that both systems perform comparably in the 4–6 Å resolution range based on Fourier-Shell correlation (FSC). In addition, by employing a recently introduced multiparticle refinement approach, we obtained a reconstruction of the EIAV CA hexamer at 2.9 Å. Our results demonstrate the potential of the new generation of energy filters and DEDs for STA, and the effects of using different processing pipelines on their STA outcomes.

Routine Collection of High-Resolution cryo-EM Datasets Using 200 KV Transmission Electron Microscope

Cryo-electron microscopy (cryo-EM) has been established as a routine method for protein structure determination during the past decade, taking an ever-increasing share of published structural data. Recent advances in TEM technology and automation have boosted both the speed of data collection and quality of acquired images while simultaneously decreasing the required level of expertise for obtaining cryo-EM maps at sub-3 Å resolutions. While most of such high-resolution structures have been obtained using state-of-the-art 300 kV cryo-TEM systems, high-resolution structures can be also obtained with 200 kV cryo-TEM systems, especially when equipped with an energy filter. Additionally, automation of microscope alignments and data collection with real-time image quality assessment reduces system complexity and assures optimal microscope settings, resulting in increased yield of high-quality images and overall throughput of data collection. This protocol demonstrates the implementation of recent technological advances and automation features on a 200 kV cryo-transmission electron microscope and shows how to collect data for the reconstruction of 3D maps that are sufficient for de novo atomic model building. We focus on best practices, critical variables, and common issues that must be considered to enable the routine collection of such high-resolution cryo-EM datasets. Particularly the following essential topics are reviewed in detail: i) automation of microscope alignments, ii) selection of suitable areas for data acquisition, iii) optimal optical parameters for high-quality, high-throughput data collection, iv) energy filter tuning for zero-loss imaging, and v) data management and quality assessment. Application of the best practices and improvement of achievable resolution using an energy filter will be demonstrated on the example of apo-ferritin that was reconstructed to 1.6 Å, and Thermoplasma acidophilum 20S proteasome reconstructed to 2.1-Å resolution using a 200 kV TEM equipped with an energy filter and a direct electron detector.

Routine Collection of High-Resolution cryo-EM Datasets Using 200 KV Transmission Electron Microscope.

Cryo-electron microscopy (cryo-EM) has been established as a routine method for protein structure determination during the past decade, taking an ever-increasing share of published structural data. Recent advances in TEM technology and automation have boosted both the speed of data collection and quality of acquired images while simultaneously decreasing the required level of expertise for obtaining cryo-EM maps at sub-3 Å resolutions. While most of such high-resolution structures have been obtained using state-of-the-art 300 kV cryo-TEM systems, high-resolution structures can be also obtained with 200 kV cryo-TEM systems, especially when equipped with an energy filter. Additionally, automation of microscope alignments and data collection with real-time image quality assessment reduces system complexity and assures optimal microscope settings, resulting in increased yield of high-quality images and overall throughput of data collection. This protocol demonstrates the implementation of recent technological advances and automation features on a 200 kV cryo-transmission electron microscope and shows how to collect data for the reconstruction of 3D maps that are sufficient for de novo atomic model building. We focus on best practices, critical variables, and common issues that must be considered to enable the routine collection of such high-resolution cryo-EM datasets. Particularly the following essential topics are reviewed in detail: i) automation of microscope alignments, ii) selection of suitable areas for data acquisition, iii) optimal optical parameters for high-quality, high-throughput data collection, iv) energy filter tuning for zero-loss imaging, and v) data management and quality assessment. Application of the best practices and improvement of achievable resolution using an energy filter will be demonstrated on the example of apo-ferritin that was reconstructed to 1.6 Å, and Thermoplasma acidophilum 20S proteasome reconstructed to 2.1-Å resolution using a 200 kV TEM equipped with an energy filter and a direct electron detector.

Accurate time zero determination in an ultrafast transmission electron microscope without energy filter

In ultrafast transmission electron microscopy, time zero can be accurately determined by making use of the photon-induced near-field electron microscopy (PINEM) effect, which causes electrons interacting with the near fields of a nanoparticle to coherently gain or lose energy in multiples of the photon energy when the laser pump and electron probe pulse overlap in time. If the instrument is not equipped with an energy filter, which is required to observe the PINEM effect, the response of a sample is frequently monitored instead. However, the gradual or delayed onset of this response can render an accurate measurement as challenging. Here, we demonstrate a simple and accurate method for determining time zero without an energy filter that is based on the observation that the outline of a nanoparticle blurs when the electron and laser pulse overlap in time. We show that this phenomenon arises from the PINEM effect, which causes some electrons to gain a large energy spread, thus blurring the image due to the chromatic aberration of the imaging system. This effect can also be used to characterize the instrument response and determine the laser polarization in situ. Furthermore, it may find applications for mapping out the near fields of a nanoparticle without the help of an energy filter.

Structure-based virtual screening workflow to identify antivirals targeting HIV-1 capsid.

We have identified novel HIV-1 capsid inhibitors targeting the PF74 binding site. Acting as the building block of the HIV-1 capsid core, the HIV-1 capsid protein plays an important role in the viral life cycle and is an attractive target for antiviral development. A structure-based virtual screening workflow for hit identification was employed, which includes docking 1.6 million commercially-available drug-like compounds from the ZINC database to the capsid dimer, followed by applying two absolute binding free energy (ABFE) filters on the 500 top-ranked molecules from docking. The first employs the Binding Energy Distribution Analysis Method (BEDAM) in implicit solvent. The top-ranked compounds are then refined using the Double Decoupling method in explicit solvent. Both docking and BEDAM refinement were carried out on the IBM World Community Grid as part of the FightAIDS@Home project. Using this virtual screening workflow, we identified 24 molecules with calculated binding free energies between − 6 and − 12 kcal/mol. We performed thermal shift assays on these molecules to examine their potential effects on the stability of HIV-1 capsid hexamer and found that two compounds, ZINC520357473 and ZINC4119064 increased the melting point of the latter by 14.8 °C and 33 °C, respectively. These results support the conclusion that the two ZINC compounds are primary hits targeting the capsid dimer interface. Our simulations also suggest that the two hit molecules may bind at the capsid dimer interface by occupying a new sub-pocket that has not been exploited by existing CA inhibitors. The possible causes for why other top-scored compounds suggested by ABFE filters failed to show measurable activity are discussed.Supplementary InformationThe online version contains supplementary material available at 10.1007/s10822-022-00446-5.

Photovoltaic Performance of Spherical TiO2 Nanoparticles Derived from Titanium Hydroxide Ti(OH)4: Role of Annealing Varying Temperature

High-quality titanium dioxide (TiO2 or titania) nanoparticles (TiO2NPs) with tailored morphologies are desirable for efficient photovoltaic applications. In this view, some thin films containing spherical TiO2NPs were prepared on indium tin oxide (ITO) and silicon (Si) substrates from titanium hydroxide Ti(OH)4 using the unified sol-gel, spray and spin coating method followed by thermal annealing at different temperatures (in the range of 200–650 °C). Samples were characterized using various analytical tools to determine the influence of annealing temperatures on their structures, morphologies, and optical and photovoltaic characteristics. A field-emission scanning electron microscope (FESEM) and energy-filtered transmission electron microscopy (EFTEM) images of the annealed films displayed the existence of spherical TiO2NPs of average size in the range of 3.2 to 33.94 nm. XRD analysis of the films showed their amorphous nature with anatase and rutile phase. Optical UV-Vis spectral analysis of the annealed films exhibited a decrease in the bandgap energy from 3.84 to 3.24 eV with the corresponding increase of annealing temperature from 200 to 650 °C. The optimum films obtained at 500 and 600 °C were utilized as electron transport layers to fabricate the metal-insulator-semiconductor solar cells. The cells’ power conversion efficiency assembled with the spherical TiO2NPs-enclosed thin films annealed at 500 and 600 °C were 1.02 and 0.28%, respectively. Furthermore, it was shown that the overall properties and photovoltaic performance of the TiO2NPs-based thin films could be improved via thermal annealing.

Recent progress and future perspective of electron cryomicroscopy for structural life sciences.

The three-dimensional structure of biological macromolecules, such as proteins and nucleic acids, and their complexes is the fundamental information not only for life sciences but also for medical sciences and drug design. Electron cryomicroscopy has become an extremely powerful tool for high-resolution structural analysis of biological macromolecules, not just in addition to X-ray crystallography and nuclear magnetic resonance sepectroscopy (NMR) that have been used as the basic techniques in structural biology. By the development of hardware and software, such as transmission electron cryomicroscopes with highly stable and controllable electron optics, cold field emission gun and energy filter, complementary metal oxide semiconductor (CMOS)-based direct electron detectors with high frame rate and high sensitivity, high-speed computers and software programs for image analysis, electron cryomicroscopy now allows structure determination of biological macromolecules at atomic levels within a few days even from a drop of solution sample with an amount as small as a few micrograms. How can the structures of macromolecules be imaged and analyzed at atomic level resolution in their native states despite their high sensitivity to radiation damage at a relatively low level of electron irradiation? We describe recent progress and future perspective of electron cryomicroscopy for structural life sciences.

An investigation of improved titanium/titanium nitride barriers for submicron aluminum-filled contacts by energy-filtered transmission electron microscopy

Abstract The adaptation of titanium/titanium nitride barriers which are commonly used for tungsten-filled contacts to aluminum-filled contacts has encountered some limitations. A main issue is the decomposition of titanium nitride manufactured by physical vapour deposition through reaction with aluminum. In this investigation two different concepts for barrier improvement have been pursued: 1. stuffing of a conventional barrier by a rapid thermal process in an oxygen-rich atmosphere and, 2. use of a barrier manufactured by chemical vapour deposition. The aim of the transmission electron microscopic analysis was to explain different electrical breakdown characteristics during thermal stressing of chips with these barriers. Energy-filtered transmission electron microscopy was used to monitor elemental distributions down to nanometer scale. Both concepts are found to improve barriers for aluminumfilled contacts.

Methods for Characterising the Precipitation of Nanometer-Sized Secondary Hardening Carbides and Related Effects in Tool Steels

AbstractNanometer-sized secondary hardening carbides are the most relevant microstructural constituents regarding the properties of tool steels. Due to their extreme fineness, direct inspection by microscopy is difficult and time consuming despite the progress recently achieved, e. g. by energy filtering transmission electron microscopy. Indirect methods are therefore additionally employed to obtain more detailed information on the processes taking place. Differential scanning calorimetry and in-situ hot hardness testing are demonstrated as powerful methods for the determination of kinetic data. In combination with results from a recently developed tensile specimen and test procedure for hard materials with low ductility, more detailed conclusions can be drawn on the effects of secondary hardening carbides on the strength and the thermal stability.