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In this report, we applied annular bright-field and annular dark-field low-energy (30 keV) scanning transmission electron microscopy imaging to a vitreous ice-embedded biological macromolecule, T4 phage, to investigate the applicability of these methods for morphological investigation and sample screening. Multiple camera lengths were examined to find the optimal acceptance angle for both modes. Image clarity differed substantially between the modes, with the presence of ice also strongly influencing the quality of acquired micrographs. In annular dark-field mode, the proper discrimination of electrons scattered by the specimen from those scattered by the background ice was found to be difficult due to the severe overlap of the scattered electrons. The resulting micrographs lacked clarity, and the ice-embedded phage particles could only be discerned after post-processing image adjustment. However, in annular bright-field mode, despite similar overlapping of the scattered electrons, it was possible to assess the morphology and intactness of the specimen in the embedding ice, suggesting that this mode may find utility in low-energy cryo-scanning transmission electron microscopy imaging methods.

In this work, we have explored the factors which govern mean free path values obtained from off-axis electron holography measurements. Firstly, we explore the topic from a theoretical perspective, and show that the mean amplitude reconstructed from off-axis holograms is due to the coherent portion of the direct, central object-transmitted beam only – it is not affected by the presence or absence of other scattered beams. Secondly, we present a detailed experimental study which compares mean free path values obtained from hologram sideband, centreband, EELS, and TEM measurements as a function of optical collection angle and energy-loss-filtering. These results confirm that the coherent portion of the direct beam defines the mean amplitude, and additionally show that the coherent portion corresponds to the conventional energy-filtered signal (with threshold 5 eV in this work). Finally, we present summary measurements from a selection of different materials, and compare the results against a simple electron scattering model. This study reinforces the claim that the mean amplitude is defined by the energy-filtered direct beam, and confirms that the contributions of elastic and inelastic scattering to the total mean free path are broadly in line with theoretical expectations for these different materials. These results in aggregate indicate that neither experimental collection angles nor enhanced sensitivity to low-loss phonon scattering affect the mean amplitude signal arising from off-axis holography reconstructions, nor the associated mean free path values which are derived from this mean amplitude.

Objectives: To understand the impact of 3-monthly treatment with paliperidone palmitate on patient management, including non-adherence and relapse, from a psychiatrist and nurse perspective for 73 patients enrolled in a patient familiarisation programme (PFP) in New Zealand. Methods: An online questionnaire was sent to clinicians with at least 6 months of regular interaction with PFP patients. Questions addressed treatment effectiveness and patient management changes. Analyses are descriptive only and do not represent patient or carer perspectives. Results: Seven psychiatrists, representing 58 of 73 (79.5%) of patients, and 17 nurses responded to the survey. Psychiatrists were satisfied with efficacy and tolerability and relapse prevention. Treatment goals were either ‘met’ (2/7; 28.6%) or ‘exceeded’ (5/7; 71.4%). The focus on adherence issues decreased and the focus on life areas and recovery goals increased. Conclusions: From the clinician perspective, 3-monthly paliperidone palmitate offers patients the potential to remain adherent and improve social functioning.

For many macromolecular complexes, the inability to uniformly disperse solubilized specimen particles within vitreous ice films precludes their analysis by cryo-electron microscopy (cryo-EM). Here, we introduce a sample preparation process using "perpetually-hydrated" graphene oxide flakes as particle support films, and report vastly improved specimen dispersion. Furthermore, we provide evidence that the presence of graphene oxide flakes in vitreous ice results in a significant reduction in electron beam-induced specimen decomposition. The new method introduced in this study incorporates hydrated graphene oxide flakes into a standard sample preparation regime, without the need for additional tools or devices, making it a cost-effective and easily adoptable alternative to currently available sample preparation approaches.

A new SEM-based in-line electron holography microscope has been under development. The microscope utilizes conventional SEM and BF-STEM functionality to allow for rapid searching of the specimen of interest, seamless interchange between SEM, BF-STEM and holographic imaging modes, and makes use of coherent low-energy in-line electron holography to obtain low-dose, high-contrast images of light element materials. We report here an overview of the instrumentation and first experimental results on gold nano-particles and carbon nano-fibers for system performance tests. Reconstructed images obtained from the holographic imaging mode of the new microscope show substantial image contrast and resolution compared to those acquired by SEM and BF-STEM modes, demonstrating the feasibility of high-contrast imaging via low-energy in-line electron holography. The prospect of utilizing the new microscope to image purified biological specimens at the individual particle level is discussed and electron optical issues and challenges to further improve resolution and contrast are considered.

Crystal diffraction is a well-established technique for high-resolution structural analysis of material science and biological samples. However, the recovered structure is a result of averaging over all the unit cells in the crystal, which smears out the imperfections, atomic defects, or asymmetries and chiral properties of the individual molecules. We propose Bragg holography, where a nano-crystal is imaged at a defocus distance allowing separation of the diffracted beams, without turning them into peaks. The presence of a reference wave gives rise to a Bragg hologram, which can be reconstructed by conventional holographic reconstruction algorithms. The recovered complex-valued wavefront contains the complete information about the atomic distribution in the crystal, including defects. Bragg holography is demonstrated for gold nano-crystals, and its feasibility for biological nano-crystals is shown.

The mean free path governing the scattering of high-energy electrons in cadmium telluride (CdTe) has been measured and analyzed using off-axis electron holography (OEH). In the first part of the study, the total mean free path value was determined via acquisition and aggregation of a large off-axis holography dataset at 300 kV and room temperature, yielding the value λ O E H = 52 ± 7 nm. This is significantly shorter than some previously reported values obtained via different experimental techniques and theoretical calculations. To confirm the validity of the measurement and to understand the underlying physical scattering processes, the study was extended to systematically investigate the role of electron energy loss, electron scattering angle, and specimen temperature in the overall holography measurement. This allowed the observed mean free path value to be clearly decomposed into terms of electronic (inelastic) and nuclear (elastic) scattering processes in the material and enabled direct measurement of the relevant contributions. Specifically, the determined attenuation coefficients were μ i n e l ( Δ E > 5 eV ) = 5.9 ± 1.2 μ m − 1 and μ e l ( Δ E 3 mrad ) = 13.5 ± 1.2 μ m − 1 (full details in the main text). With appropriate consideration of the relevant scattering mechanisms, the mean free path value determined here from off-axis holography measurements is consistent with prior experimental measurements from other techniques and theoretical calculations. These insights and measurements should be of future value for quantitative holography and electron beam scattering experiments in CdTe.

We utilized gas-phase condensation to deposit size-selected Pd nanoparticles (NPs) on Mg nanofilms and systematically studied the catalytic conversion to localized MgH2 nanodomains upon exposure to hydrogen. Atomic force microscopy (AFM), aberration corrected transmission electron microscopy (TEM), and electron energy-loss spectroscopy (EELS) experiments were applied to map localized embryonic hydride nanodomains protruding from the Mg surface as a function of hydrogenation time, NP surface coverage, applied hydrogen pressure, and NP size. The results show that Pd NPs dissociate hydrogen and create atomic hydrogen pathways for hydrogenating the Mg nanofilm. The Pd NPs also inhibit oxidation of the underlying Mg nanofilm. Interestingly, the Mg nanofilm could be fully hydrogenated with a small quantity of Pd NPs at room temperature and modest hydrogen pressures. The localized hydrogenation enables improved control over the spatial distribution of hydride nanodomains making this configuration promising for future on-board hydrogen storage applications.

Competition-related dietary intake has not yet been investigated in Gaelic football. The present study examined the precompetition macronutrient intake of elite male Gaelic football players. Forty players from two teams completed a food diary on the 2 days preceding competition (Day 1 and Day 2) and on the match day prior to the match (match day). Carbohydrate intake was significantly greater on Day 2 compared with Day 1, for both absolute (295 ± 98 vs. 318 ± 77 g;p = .048; −23.6 g, 95% confidence interval [−47.3, 0.2]; Cohen’sd = 0.27) and relative intake (3.4 ± 1.1 vs. 3.7 ± 1.0 g/kg;p = .027; −0.3 g/kg, 95% confidence interval [−0.6, −0.03]; Cohen’sd = 0.32). The number of players in accordance with and not in accordance with the guidelines for carbohydrate intake on Day 2 was significantly different to an expected frequency distribution, χ2(1) = 32.400;p ≤ .001; φ = 0.9, with a greater number of players not meeting the guidelines (observedN = 2 vs. 38). The number of players in accordance with and not in accordance with the recommendations for carbohydrate intake on match day was significantly different to an expected frequency distribution, χ2(1) = 8.100;p = .004; φ = 0.45, with a greater number of players meeting the guidelines (observedN = 29 vs. 11). The major finding from the current investigation was that a significantly greater number of players did not meet carbohydrate intake guidelines on the day before competition. Individualized nutritional interventions are required in order to modify the current prematch dietary intake.

We report on the design and synthesis of high performance catalytic nanoparticles with a robust geometry via magnetron-sputter inert-gas condensation. Sputtering of Pd and Mg from two independent neighbouring targets enabled heterogeneous condensation and growth of nanoparticles with controlled Pd core-MgO porous shell structure. The thickness of the shell and the number of cores within each nanoparticle could be tailored by adjusting the respective sputtering powers. The nanoparticles were directly deposited on glassy carbon electrodes, and their catalytic activity towards methanol oxidation was examined by cyclic voltammetry. The measurements indicated that the catalytic activity was superior to conventional bare Pd nanoparticles. As confirmed by electron microscopy imaging and supported by density-functional theory (DFT) calculations, we attribute the improved catalytic performance primarily to inhibition of Pd core sintering during the catalytic process by the metal-oxide shell.

We report efficient design and facile synthesis of size-tunable organic/inorganic nanosheets, via a straightforward liquid exfoliation-adsorption process, of a near percolating gold (Au) thin film deposited onto a branched polyethylenimine (bPEI) matrix. The nanosheets are stiff enough to sustain their two-dimensional (2D) nature in acidic conditions, yet flexible enough to undergo a perfect reversible shape transformation to 1D nanoscrolls in alkaline conditions. The shape transformations, and associated optical property changes, at different protonation states are monitored by transmission electron microscopy (TEM), atomic force microscopy (AFM), UV-visible spectroscopy and zeta potential measurements. Because of their large surface area, both nanosheets and nanoscrolls could be used as capturing substrates for surface-enhanced Raman scattering (SERS) applications.

Heterogeneous gas-phase condensation is a promising method of producing hybrid multifunctional nanoparticles with tailored composition and microstructure but also intrinsically introduces greater complexity to the nucleation process and growth kinetics. Herein, we report on the synthesis and growth modeling of silicon–silver (Si–Ag) hybrid nanoparticles using gas-aggregated cosputtering from elemental Si and Ag source targets. The final Si–Ag ensemble size was manipulated in the range 5–15 nm by appropriate tuning of the deposition parameters, while variations in the Si–Ag sputtering power ratio, from 1.8 to 2.25, allowed distinctive Janus and core–satellite structures, respectively, to be produced. Molecular dynamics simulations indicate that the individual species first form independent clusters of Si and Ag without significant intermixing. Collisions between unlike species are unstable in the early stages of growth (

Cryo-electron microscopy (cryo-EM) has become the method of choice in the field of structural biology, owing to its unique ability to deduce structures of vitreous ice-embedded, hydrated biomolecules over a wide range of structural resolutions. As cryo-transmission electron microscopes (cryo-TEM) become increasingly specialised for high, near-atomic resolution studies, operational complexity and associated costs serve as significant barriers to widespread usability and adoptability. To facilitate the expansion and accessibility of the cryo-EM method, an efficient, user-friendly means of imaging vitreous ice-embedded biomolecules has been called for. In this study, we present a solution to this issue by integrating cryo-EM capabilities into a commercial scanning electron microscope (SEM). Utilising the principle of low-energy in-line electron holography, our newly developed hybrid microscope permits low-to-moderate resolution imaging of vitreous ice-embedded biomolecules without the need for any form of sample staining or chemical fixation. Operating at 20 kV, the microscope takes advantage of the ease-of-use of SEM-based imaging and phase contrast imaging of low-energy electron holography. This study represents the first reported successful application of low-energy in-line electron holographic imaging to vitreous ice-embedded small biomolecules, the effectiveness of which is demonstrated here with three morphologically distinct specimens.

Porous films of tantalum (Ta) and its oxides exhibit numerous properties suitable for high surface area applications, mainly in the semiconductor and bio-implant industries. Such films can be developed by Ta nanoparticle deposition using DC magnetron sputtering with gas aggregation. In order to engineer films of desirable properties, accurate control and in-depth understanding of the processes and parameters of nanoparticle growth, deposition and coalescence are crucial. Of utmost importance is to control the film’s porosity, since it determines many of the other physical properties. To this end, we performed a number of classical Molecular Dynamics simulations to study the coalescence of two or more Ta nanoparticles. Temperature, relative size and crystallographic orientation, defect content, degree of crystallinity and deposition rate effects were taken into account, and a mapping of the sintering processes was acquired. A broad range of possible interaction mechanisms were observed, from simple nanoparticle reorientation in order to achieve epitaxial configuration, to atomic adsorption, neck formation, twinning within the nanoparticles and full consolidation into a single, larger nanoparticle. The parameters studied are directly linked to experimental deposition parameters; therefore, fitting them accordingly can lead to growth of films with bespoke properties.

Low-temperature plasma activated wafer bonding is an important technology for the 3D integration of semiconductor devices, such as sensors and CMOS devices integrated on opposite sides on the same chip. In a volume production environment, monitoring the bond strength is essential to the overall product quality. In this publication, commonly used methods for bond strength measurement and their relative advantages and disadvantages for quality control are compared with a novel technique of sample preparation for tensile testing.

Tantalum nanoparticle (NP) films have been deposited on silicon substrates, using sputter deposition with gas aggregation. The resultant NP films have been characterized using high resolution atomic force microscopy and X-ray fluorescence spectroscopy. The films remain stable and the NPs maintain a spherical structure on annealing up to 600 °C. In addition to characterization, these NP films have been locally patterned by atomic force microscope scanning of the surface in contact mode.

Vertical integration of diverse semiconductor technologies can be achieved by utilizing interconnections through entire silicon substrates, known as through silicon vias (TSVs). TSVs present an interesting case study for reliability evaluation, given the particular fabrication technologies, geometries, and potential failure modes associated with such structures. A specific TSV technology is introduced, and key parameters for reliability assessment, such as residual stress, resistance, leakage, and dielectric breakdown, are discussed. Reliability data are presented, including the characterization of TSV parameters as a function of various accelerated lifetime stress tests, as well as assessments of the density and impact of TSV manufacturing defects. The presented data demonstrate that while the TSV is inherently quite robust, latent manufacturing defects pose a significant risk to long-term reliability. Screening methodologies, defect modes, failure analysis methods, process improvement, and correspondingly improved defect density results are discussed. The results are considered pertinent to the development and reliability of novel 3-D integrated process technologies.

Infra-red photoemission microscopy has been applied for the localization of defects in 3D integrated circuits containing Through Silicon Vias (TSVs). For these investigations, the familiar (planar) emission microscopy configuration was extended to allow imaging and emission microscopy on vertical TSV sidewalls, from versatile 3D viewpoints. Flexible viewing orientation was achieved by introducing an additional reflecting surface into the optical path. Precise alignment of the angle of incidence at the air–silicon interface, with sufficient accuracy to ensure no problematic refraction-related errors, was possible using this experimental set-up. Three examples are presented, showing defect localizations and underlying physical leakage mechanisms in TSV structures.

We report on conductometric gas sensors based on single CuO nanowires and compare the carbon monoxide (CO) sensing properties of pristine as well as Pd nanoparticle decorated devices in humid atmosphere. Magnetron sputter inert gas aggregation combined with a quadrupole mass filter for cluster size selection was used for single-step Pd nanoparticle deposition in the soft landing regime. Uniformly dispersed, crystalline Pd nanoparticles with size-selected diameters around 5 nm were deposited on single CuO nanowire devices in a four point configuration. During gas sensing experiments in humid synthetic air, significantly enhanced CO response for CuO nanowires decorated with Pd nanoparticles was observed, which validates that magnetron sputter gas aggregation is very well suited for the realization of nanoparticle-functionalized sensors with improved performance.

We analyze the fundamental process of crystallization of silicon nanoclusters by means of molecular dynamics simulations, complemented by magnetron-sputter inert gas condensation, which was used to synthesize polycrystalline silicon nanoclusters with good size control. We utilize two well-established Si interatomic potentials: the Stillinger-Weber and the Tersoff III. Both the simulations and experiments show that upon cooling down by an Ar gas thermal bath, initially liquid, free-standing Si nanocluster can grow multiple crystal nuclei, which drive their transition into polycrystalline solid nanoclusters. The simulations allow detailed analysis of the mechanism, and show that the crystallization temperature is size-dependent and that the probability of crystalline phase nucleation depends on the highest temperature the cluster reaches during the initial condensation and the cooling rate after it.

We have performed open cell transmission electron microscopy experiments through pure water vapor in the saturation pressure regime (>0.6 kPa), in a modern microscope capable of sub-Å resolution. We have systematically studied achievable pressure levels, stability and gas purity, effective thickness of the water vapor column and associated electron scattering processes, and the effect of gas pressure on electron optical resolution and image contrast. For example, for 1.3 kPa pure water vapor and 300kV electrons, we report pressure stability of ± 20 Pa over tens of minutes, effective thickness of 0.57 inelastic mean free paths, lattice resolution of 0.14 nm on a reference Au specimen, and no significant degradation in contrast or stability of a biological specimen (M13 virus, with 6 nm body diameter). We have also done some brief experiments to confirm feasibility of loading specimens into an in situ water vapor ambient without exposure to intermediate desiccating conditions. Finally, we have also checked if water experiments had any discernible impact on the microscope performance, and report pertinent vacuum and electron optical data, for reference purposes.

Mean inner potential is a fundamental material parameter in solid state physics and electron microscopy and has been experimentally measured in CdTe, a technologically important semiconductor. As a first step, the inelastic mean free path for electron scattering in CdTe was determined, using electron energy loss spectroscopy, to enable precise thickness mapping of thin CdTe lamellae. The obtained value was λi(CdTe, 300 kV) = 192 ± 10 nm. This value is relatively large, given the high density of the material, and is discussed in the text. Next, electron diffraction and specimen tilting were employed to identify weakly diffracting lattice orientations, to enable the straightforward measurement of the electron phase shift. Finally, electron holography was utilized to quantitatively map the phase shift experienced by electron waves passing through a CdTe crystal, with several different propagation vectors. Utilization of both thickness and phase data allowed computation of mean inner potential as V0 (CdTe) = 14.0 ± 0.9 V, within the range of previous theoretical estimates.

Palladium nanoparticles offer an attractive alternative to bulk palladium for catalysis, hydrogen storage and gas sensing applications. Their performance depends strongly on surface structure; therefore, nanoparticle coalescence can play an important role, as it determines the resultant structure of the active sites where reactions (e.g. catalysis) actually take place, i.e. facets, edges, vertices or protrusions. With this in mind, we performed classical molecular dynamics (MD) simulations and magnetron-sputtering inert gas condensation depositions of palladium nanoparticles, supported by high-resolution transmission electron microscopy (HRTEM), to study the mechanisms that govern their coalescence. Surface energy minimisation drove the interactions initially, leading to the formation of an interface/neck, as expected. Intriguingly, at a later stage, atomic rearrangements triggered a crystallisation wave propagating through the amorphous nanoparticles, leading to mono- or polycrystalline fcc structures. In the case of crystalline nanoparticles, almost-epitaxial alignment occurred and the formation of twins and surface protrusions were observed.

Functionally graded materials offer a way to improve the physical and chemical properties of thin films and coatings for different applications in the nanotechnology and biomedical fields. In this work, design and assembly of nanoporous tantalum films with a graded oxidation profile perpendicular to the substrate surface are reported. These nanoporous films are composed of size-selected, amorphous tantalum nanoparticles, deposited using a gas-aggregated magnetron sputtering system, and oxidized after coalescence, as samples evolve from mono- to multi-layered structures. Molecular dynamics computer simulations shed light on atomistic mechanisms of nanoparticle coalescence, which govern the films porosity. Aberration-corrected (S) TEM, GIXRD, AFM, SEM, and XPS were employed to study the morphology, phase and oxidation profiles of the tantalum nanoparticles, and the resultant films. Design and assembly of tantalum nanoparticle porous films with a graded oxidation profile perpendicular to the substrate surface were fabricated by magnetron-sputter inert-gas aggregation system. At the top-most layers of the film, the larger free-surface areas of nanoparticles enable the formation of thermodynamically stable Ta2O5.

Silicon (Si) nanoparticles were coated inflight with silver (Ag) atoms using a novel method to prepare multicomponent heterostructured metal-semiconductor nanoparticles. Molecular dynamics (MD) computer simulations were employed, supported by high-resolution bright field (BF) transmission electron microscopy (HRTEM) and aberration-corrected scanning transmission electron microscopy (STEM) with a resolution ≤0.1 nm in high angle annular dark field (HAADF) mode. These studies revealed that the alloying behavior and phase dynamics during the coating process are more complex than when attaching hetero-atoms to preformed nanoparticles. According to the MD simulations, Ag atoms condense, nucleate and diffuse into the liquid Si nanoparticles in a process that we term “inoculation”, and a phase transition begins. Subsequent solidification involves an intermediate alloying stage that enabled us to control the microstructure and crystallinity of the solidified hybrid heterostructured nanoparticles.

Physical vapor deposition, in combination with gas-aggregation (PVD-GA), is a controllable method for creation of diverse nanoparticle structures. Given the size effects that dominate the physics of nanoparticles, a particular advantage of the PVD-GA technique is the compatibility with in situ mass filtering of the nanocluster beam.In the current work, PVD-GA has been utilized to deposit Ag and Si nanoparticles. Nanoparticles were analyzed using in situ quadrupole mass spectrometry (charge/mass ratio), atomic force microscopy (nanoparticle height), and transmission electron microscopy (nanocluster diameter & crystallinity). The results for particle size distribution were cross-correlated, with excellent agreement.Different growth methods & conditions were explored, resulting in controlled differences in the measured particle size distributions and surface coverage. A novel growth configuration utilizing a conventional sputter source in combination with a linear magnetron allowed a significant (fivefold) increase in Ag cluster yield.

Through Silicon Via (TSV) technology, to serve as electrical connection between metallization layers on the front and backside of the same wafer, has been developed by austriamicrosystems AG. During the development phase, defects were found that could be assigned to an established defect type known as “contact liner volcano”. To our knowledge this is the first time that such a volcano formation is reported from the inside of a TSV.

Today 3D interconnection approaches are considered to provide one of the most promising enabling technologies for “More than Moore” solutions. In particular, 3D integration can provide significant progress in semiconductor device development regarding increased system functionality and integration density. In this paper, we describe an innovative concept for sensor integration based on a quality-proven “open” TSV technology on the basis of a 0.35μm CMOS process. An application-optimized sensor-layer is processed on a specific wafer substrate, whereas the CMOS circuits of the system can remain cost-efficiently on an appropriate 0.35μm CMOS or HV-CMOS technology. Another advantage of the proposed TSV solution is the geometric aspect. As the CMOS is attached to the sensor backside, almost 100% of the chip area can be used for the sensing functionality. In the presented technological approach, the sensor wafer is finalized with processing a top metal layer and successive bond oxide layers. The bond oxide layers are planarized by chemo mechanical polishing (CMP). The CMOS wafer is fabricated using a regular 0.35μm CMOS technology up to the vias before the last metal layer. A nitride layer is deposited in order to protect the integrated circuits from damages during the back grinding process. Prior to bonding, the CMOS wafer is thinned down to a thickness of 250μm and then bonded to the sensor wafer by plasma activated bonding followed by an annealing step to reinforce the bond strength. TSV etching is sequentially performed in three steps: firstly, the oxide of inter-metal dielectrics is opened. Secondly, the bulk silicon of the CMOS wafer is etched using a deep reactive ion etch (DRIE) process selectively stopping on the bond oxide of the sensor wafer. After several cleaning steps the spacer oxide is deposited followed by the spacer and bond oxide etching. For TSV metallisation, Tungsten as deposited in a CVD process is chosen providing uniform conformal coating inside the open TSVs. A sputtered Al forms the top metal and a subsequently produced passivation layer completes the fabrication process. With respect to the photo-lithography process for patterning the top metal and passivation layers, a specifically developed resist spray coating technique is used. This allows protecting the TSVs from damage due to the etching gases. The higher complexity of the lithography is compensated by a more simple and reliable processing regarding the TSV quality. The presented technological flow results in advantageous electrical properties of the TSV interconnects, e.g. low resistivity and a high breakdown voltage combined with excellent inherent reliability. The fabricated sensor devices were characterized by a variety of analytical techniques that have specifically been adapted to the requirements of 3D integrated wafer-bonded systems with TSVs. This approach allowed isolating, localizing and characterizing process related inhomogeneities and potential defects inside the open TSVs and in the wafer bond interface with improved analysis throughput. Electrical shorts of the TSV sidewall metallization to the Si substrate could be identified by Lock-in Thermography (LIT). The exact defect position at the sidewall could be estimated by applying a new defocusing technique to additionally determine the defect depth inside the TSV. As a consequence, the identified sidewall defects could subsequently be analyzed by high resolution transmission electron microscopy (HR TEM) to reveal their root causes. Scanning Acoustic Microscopy (SAM) with improved signal analysis and data evaluation was applied to identify and characterize local delamination defects in the wafer-bonded interface of the 3D sensor. The achieved progress regarding failure analysis methodology supported the technological developments and will contribute to secure quality and yield of 3D integrated devices during future manufacturing.

Topography and Deformation Measurement and FE Modeling were applied for characterization of the warpage vs. temperature behavior of several different die stacks, with or without Through Silicon Vias, for sample temperatures from 25°C…250°C. The warpage behavior is of fundamental importance for the lifetime and reliability expectation of the stack.

Depth-resolved IR photoemission microscopy was applied for localization of defects causing leakage currents within Through Si Vias (TSVs). Specifically, analyses of the changes in intensity and spatial distribution of the detected emission, as a function of the focal plane position, allow quantification of the depth of defects within the TSV. Physical failure analysis verified the presence of the defects at the coordinates specified by emission microscopy, and allowed defect failure mechanisms to be identified.

This paper is concerned with characterization and failure analysis challenges posed by 3D integration of semiconductor devices, with a particular focus on wafer bonded components and Through Silicon Vias (TSV). Requirements for sample preparation are discussed, along with advantages and limitations exhibited by various different techniques. Analysis examples with real devices are presented, along with successful sample preparation solutions enabled by a precision polishing toolset.

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In this paper we will introduce novel methodical approaches for material and failure analysis of 3D integrated devices. The potential and advantages of the new concepts and tools will be demonstrated for flip-chip-like interconnects but in addition, for the first time, for Through Silicon Vias (TSV). The employed techniques combine non-destructive fault localization with efficient and accurate target preparation to get access for following microstructure diagnostics, forming a subsequent failure analysis workflow. The concept presented here involves the application of improved Lock-In Thermography (LIT), and three different innovative concepts of high rate Focused Ion Beam (FIB) techniques.