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Ge-rich Ge2Sb2Te5 (GGST) is considered as one of the best candidates for industrial phase change memory production. GGST memory cells are generally embedded with Si or Ti nitride layers to prevent oxidation, as it leads to an undesired decrease of the GGST crystallization temperature. Furthermore, GGST films are usually doped with elements such as N, C, O, or Bi, aiming to delay GGST crystallization during the fabrication process as well as during memory cell operation. In this work, ultrahigh vacuum thermal desorption spectroscopy (TDS) was performed during isochronal annealing of a N-doped GGST film covered by a 10 nm-thick TiN x layer. Desorption is observed before GGST crystallization, but the comparison between TDS and in situ x-ray diffraction measurements shows that the main desorption peak, observed between 653 K and 703 K, occurs after GGST full crystallization. The most prominent desorbing species are Ar, N2, H2, and H. These results show that the TiN x polycrystalline layer cannot prevent N atoms from leaving the GGST layer during annealing, suggesting a progressive change of the N-doped GGST chemical composition during thermal annealing and crystallization. [ABSTRACT FROM AUTHOR]

Simulation of atomic redistribution in Geâ€"Sbâ€"Te (GST)-based memory cells during SET/RESET cycling is needed in order to understand GST memory cell failure and to design improved non-volatile memories. However, this type of atomic scale simulations is extremely challenging. In this work, we propose to use a simplified GST system in order to catch the basics of atomic redistribution in Ge-rich GST (GrGST) films using atomistic kinetic Monte Carlo simulations. Comparison between experiments and simulations shows good agreements regarding the influence of Ge excess on GrGST crystallization, as well as concerning the GST growth kinetic in GrGST films, suggesting the crystallized GST ternary compound to be off-stoichiometric. According to the simulation of atomic redistribution in GrGST films during SET/RESET cycling, the film microstructure stabilized during cycling is significantly dependent of the GST ternary phase stoichiometry. The use of amorphous layers exhibiting the GST ternary phase stoichiometry placed at the bottom or at the top of the GrGST layer is shown to be a way of controlling the microstructure evolution of the film during cycling. The significant evolution of the local composition in the amorphous solution during cycling suggests a non-negligible variation of the crystallization temperature with operation time. [ABSTRACT FROM AUTHOR]

As of 45 nm node, ultralow k (ULK) materials ([variant_greek_epsilon]r < 2.55) are widely used in microelectronic interconnects to reduce signal propagation delay. In order to get such low dielectric constant, most of these ULK are obtained using subtractive method: after co-deposition of matrix and porogen a UV cure process is used to remove labile species (porogen). During this process, porosity is created and films are densified as shrinkage increases. This paper presents an in-depth study of the UV cure process. Two kinetic models are presented to describe shrinkage rate: the nth order and the autocatalytic model. These models also used to describe photo-polymerization shrinkage-strain of dental composite, gives predictions that are in good agreement with experimental data. We find that nth-order model is best suited to describe ULK transformations during UV cure process. CHx bonds loss and carbon content can also be modeled using same kinetic model. In order to be able to build the model, initial SiOCH-CxHy film has to be over-cured to determine the maximum conversion that film can reach when submitted to extra-long cure times. Results show that such SiOCH materials have to be cured more than 250 times their nominal cure time to reach maximum shrinkage (∼50%) and a complete loss of carbon, making them looking like SiO2. When structural changes are observed at different temperature, activation energy of reactions can be determined. In this way, shrinkage reaction has an activation energy close to 1000-1100 kJ/mol and CHx bonds or carbon loss reactions have activation energy in the range of 250-400 kJ/mol, which is pretty close to C-H binding energy. [ABSTRACT FROM AUTHOR]

In this paper, we investigate the tendency of porous low-K dielectrics (also named Ultra Low-K, ULK) behavior to shrink when exposed to the electron beam of a scanning electron microscope. Various experimental electron beam conditions have been used for irradiating ULK thin films, and the resulting shrinkage has been measured through use of an atomic force microscope tool. We report the shrinkage to be a fast, cumulative, and dose dependent effect. Correlation of the shrinkage with incident electron beam energy loss has also been evidenced. The chemical modification of the ULK films within the interaction volume has been demonstrated, with a densification of the layer and a loss of carbon and hydrogen elements being observed. [ABSTRACT FROM AUTHOR]

Highlights • Copper pillars are imaged using 6 different 3D imaging techniques. • 3rd generation synchrotron beamlines and lab equipments are assessed. • A new sample preparation for synchrotron tomography is successfully tested. • The final volumes are compared, based on image quality and analysis time. Abstract In microelectronics, recently developed 3D integration offers the possibility to stack the dice or wafers vertically instead of putting their different parts next to one another, in order to save space. As this method becomes of greater interest, the need for 3D imaging techniques becomes higher. We here report a study about different 3D characterization techniques applied to copper pillars, which are used to stack different dice together. Destructive techniques such as FIB/SEM, FIB/FIB, and PFIB/PFIB slice and view protocols have been assessed, as well as non-destructive ones, such as laboratory-based and synchrotron-based computed tomographies. A comparison of those techniques in the specific case of copper pillars is given, taking into account the constraints linked to the microelectronics industry, mainly concerning resolution and sample throughput. Laboratory-based imaging techniques are shown to be relevant in the case of punctual analyses, while synchrotron based tomographies offer highly resolved volumes for larger batches of samples. [ABSTRACT FROM AUTHOR]

X-ray tomography is widely used in materials science. However, X-ray scanners are often based on polychromatic radiation that creates artifacts such as dark streaks. We show this artifact is not always due to beam hardening. It may appear when scanning samples with high-Z elements inside a low-Z matrix because of the high-Z element absorption edge: X-rays whose energy is above this edge are strongly absorbed, violating the exponential decay assumption for reconstruction algorithms and generating dark streaks. A method is proposed to limit the absorption edge effect and is applied on a microelectronic case to suppress dark streaks between interconnections. [ABSTRACT FROM AUTHOR]

Total variation minimization is applied to the particular case of X-ray tomography in a scanning electron microscope. To prove the efficiency of this reconstruction method, noise-free and noisy data based on the Shepp & Logan phantom have been simulated. These simulations confirm that Total variation minimization-reconstruction algorithm better manages data containing low number of projections with respect to simultaneous iterative reconstruction technique or filtered backprojection, even in the presence of noise. The algorithm has been applied to real data sets, with a low angular sampling and a high level of noise. Two samples containing micro-interconnections have been analyzed and 3D reconstructions show that Total variation minimization-based algorithm performs well even with 60 projections in order to properly recover a 500 nm diameter void inside a copper interconnection. [ABSTRACT FROM AUTHOR]

Highlights: [•] X-ray tomography in a SEM is efficient for 3D integration in microelectronics. [•] Employing thin metal targets as X-ray source increases the scanner resolution. [•] A 3D resolution pattern has been created by using a plasma FIB. [•] The 3D resolution of the instrument is proved to be about 500nm at 8.4keV. [Copyright &y& Elsevier]

Abstract: A new STEM XEDS tomography technique is proposed thanks to the implementation of multi EDX SDD detectors in analytical TEMs. The technique flow is presented and the first results obtained on a 28nm FDSOI transistor are detailed. The latter are compared with 2D XEDS analysis to demonstrate the interest of the slice extraction in all directions from a large analyzed volume without any 3D overlap effect issues. [Copyright &y& Elsevier]

Three-dimensional focused ion beam/scanning electron microscopy (FIB/SEM tomography) is currently an important technique to characterize in 3D a complex semiconductor device or a specific failure. However, the industrial context demands low turnaround time making the technique less useful. To make it more attractive, the following study focuses on a specific methodology going from sample preparation to the final volume reconstruction to reduce the global time analysis while keeping reliable results. The FIB/SEM parameters available will be first analyzed to acquire a relevant dataset in a reasonable time (few hours). Then, a new alignment strategy based on specific alignment marks [using tetraethoxylisane (TEOS) and Pt deposition] is proposed to improve the volume reconstruction speed. These points combined represent a considerable improvement regarding the reliability of the results and the time consumption (gain of factor 3). This method is then applied to various case studies illustrating the benefits of the FIB/SEM tomography technique such as the precise identification of the origin of 3D defects, or the capability to perform a virtual top-down deprocessing on soft material not possible by any mechanical solution. [ABSTRACT FROM AUTHOR]

Examines the distribution of an inverted ferroelectric domains on the periodically poled KTA single crystal. Use of an X-ray diffraction setup; Availability of a coherent beams at the third-generation synchrotron source; Phase difference of the diffracted waves.

In situ transmission electron microscopy (TEM) observations were performed for a better understanding of the 'melt quenched' GeTe crystallization mechanism. The evolution of the crystallite morphology observed during annealing shows a growth-dominated crystallization behavior. Scanning transmission electron microscopy-electron dispersive x-ray spectroscopy and high resolution electron microscopy experiments were also performed on cycled GeTe devices, showing that void formation is responsible for the cell failure after 107 cycles. [ABSTRACT FROM AUTHOR]

While microelectronic devices are frequently characterized with surface-sensitive techniques having nanometer resolution, interconnections used in 3D integration require 3D imaging with high penetration depth and deep sub-micrometer spatial resolution. X-ray tomography is well adapted to this situation. In this context, the purpose of this study is to assess a versatile and turn-key tomographic system allowing for 3D x-ray nanotomography of copper pillars. The tomography tool uses the thin electron beam of a scanning electron microscope (SEM) to provoke x-ray emission from specific metallic targets. Then, radiographs are recorded while the sample rotates in a conventional cone beam tomography scheme that ends up with 3D reconstructions of the pillar. Starting from copper pillars data, collected at the European Synchrotron Radiation Facility, we build a 3D numerical model of a copper pillar, paying particular attention to intermetallics. This model is then used to simulate physical radiographs of the pillar using the geometry of the SEM-hosted x-ray tomography system. Eventually, data are reconstructed and it is shown that the system makes it possible the quantification of 3D intermetallics volume in copper pillars. The paper also includes a prospective discussion about resolution issues. [ABSTRACT FROM AUTHOR]

Two stroboscopic shutters, adapted for the study of periodic phenomena in the 1–400 Hz range, were developed and tested. The principle, advantages and drawbacks of these devices are pointed out. Results obtained by x-ray diffraction imaging (topography) on a vibrating silicon crystal, and on the investigation of defects produced in KTiOPO4 by the application of an electric field, illustrate the possibilities of this stroboscopic imaging technique at low frequencies. [ABSTRACT FROM AUTHOR]

The spatial resolution and the indexing quality obtained with an automated orientation and phase mapping tool are analyzed for different Transmission Electron Microscope (TEM) illumination settings. The electron probe size and convergence angle are studied for two TEM configuration modes referred as microprobe and nanoprobe modes. Using a 10 μm C 2 aperture in a FEI Tecnai F20 (S)TEM, the nanoprobe mode is used to get a small convergent electron beam while the microprobe mode provides a nearly parallel illumination at the cost of a larger probe size. The nanoprobe configuration enables to increase the spatial resolution (∼1 nm vs 3 nm) but also affects the fraction of mis-indexed points (15% vs 1%). Indexing errors are attributed to the increase by a factor of three of the convergence angle with respect to the microprobe mode. While intermediate optimum settings may be found and are potentially achievable on electron microscopes providing a ‘free lens’ control or a larger choice of C 2 apertures, it is emphasized that the spatial resolution cannot be considered without reference to the indexing quality and, consequently to the convergence angle. [ABSTRACT FROM AUTHOR]

Abstract: In this paper, reliability of Through Silicon via (TSV) interconnects is analyzed for two technologies. First part presents an exhaustive analysis of Cu TSV-last approach of 2μm diameter and 15μm of depth. Thermal cycling and electromigration stresses are performed on dedicated devices. Thermal cycling is revealed to induce only defects on non-mature processes. Electromigration induces voids in adjacent metal level, right at TSV interface. Moreover, the expected lifetime benefit by increasing line thickness does not occur due to increasing dispersion of voiding mechanism. Second part covers reliability of Cu TSV-middle technology, of 10μm diameter and 80μm depth, with thermal cycling, BEoL dielectric breakdown, and electromigration study. Thermal cycling is assessed on two designs: isolated and dense TSV patterns. Dielectric breakdown tests underline an impact of TSV on the reliability of metal level dielectrics right above TSV. Electromigration reveal similar degradation mechanism and kinetic as on TSV-last approach. [Copyright &y& Elsevier]