Terahertz heterodyne spectrometer instruments have been traditionally limited to a single pixel or a handful of pixels due to integration and assembly constraints and a limited availability of local oscillator (LO) power. As a solution we propose a novel silicon-micromachined planar and modular packaging strategy, that will allow for a dense integration of a large number of pixels. Moreover, the RF- and LO signals will be quasi-optically coupled via two identical but opposite lens arrays, such that a single LO-source can efficiently pump all HEB-mixers of the 2x2 pixel demonstrator array simultaneously. This work reports on an intermediate step, where we validate the lens array performance and LO power coupling efficiency, by slightly modifying the silicon package into a transmit array configuration. In this way, the LO power coupled into the stack is directly reradiated on the other side, which is then measured using a liquid helium cooled bolometer.@en

The authors regret that the original graphical abstract contained an error by accident. In particular, the values of the OH density for the calcined SBA-15 and solvent-&-Fenton-treated SBA-15 were swapped. These values contradict the main message of the study. The values contained in the paper are however correct. In summary, the paper's data are correct but the graphical abstract contained swapped data leading to a contradiction. Below, an amended graphical abstract can be found, as well as in the online journal website. The authors would like to apologise for any inconvenience caused. [Figure presented]

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Hafnia-based thin films exhibit unconventional ferroelectricity. These materials also show rich polymorphism, and thus temperature and field-driven phase transitions, as well as oxygen migration. In a bigger context of exploring the synergy between ferroelectricity and diffusion-based structural phenomena, here we study temperature-dependent phase transitions in epitaxial Hf0.5Zr0.5O2(HZO)/La0.67Sr0.33MnO3 (LSMO, bottom electrode) heterostructures. We report topotactic phase transitions and their clear pathways in both LSMO and HZO layers upon heating under vacuum, using in situ scanning transmission electron microscopy (STEM). Specifically, we directly image oxygen and cationic columns using integrated differential phase contrast STEM and follow their evolution with temperature. We also perform in situ high temperature X-ray diffraction in air and show that the LSMO layer undergoes reversible thermal expansion and contraction when heated up to 850 °C, whereas HZO undergoes strain relaxation beyond 750 °C without any reversible phase transition. Our results provide a comprehensive and direct understanding of temperature-dependent structure, defect, and property correlations in these systems.

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A cold-rolled Ti-V high strength low alloy (HSLA) steel was isothermally annealed at 650 °C and 700 °C for different times. A unique combination of techniques including visible light microscopy (VLM), transmission electron microscopy (TEM), matrix dissolution, small angle neutron scattering (SANS) and hardness measurement has been employed to investigate the evolution of microstructure, hardness and precipitate composition, size and volume fraction. Results show that recrystallization is completed after annealing 8 h at 650 °C and 30 min at 700 °C. Three types of precipitates were identified: large Ti(C,N), medium-size (Ti,V)(C,N) and small (Ti,V)C. The Ti/(Ti+V) atomic ratio in the (Ti,V)C precipitates decreases with increasing radius in the 1–15 nm range, which can be explained by the initial nucleation of a TiC-rich core. The average size of the (Ti,V)C precipitates increases, whereas the number density decreases during annealing. The volume fractions of the three types of precipitates were separately determined by the matrix dissolution method. The volume fractions of (Ti,V)C precipitates obtained by matrix dissolution are comparable even slightly more accurate than those obtained by SANS. The hardness first increases and then decreases when annealing at both temperatures, which can be correlated well with the observed microstructural and precipitate evolution.

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Magnesium thin films covered with a layer of Pd absorb hydrogen at much higher pressures than bulk Mg. Such an effect was originally explained as a consequence of elastic clamping on Mg by the capping Pd layer. An alternative interpretation later suggested that the pressure increase could originate from simple alloying between Mg and Pd. Here we resolve this controversy by measuring the hydrogenation and dehydrogenation isotherms of Mg-Pd thin film alloys over a wide range of compositions. Our results disentangle the effects of elastic clamping and alloying and highlight the role of plastic deformations.

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The alloys (GeTe)_x(AgSbTe₂)_100-x, commonly known as TAGS-x, are among the best performing p-type thermoelectric materials for the composition range 80 ≤ x ≤ 90 and in the temperature range 200-500 °C. They adopt a rhombohedrally distorted rocksalt structure at room temperature and are reported to undergo a reversible phase transition to a cubic structure at ∼250 °C. However, we show that, for the optimal x = 85 composition (TAGS-85), both the structural and thermoelectric properties are highly sensitive to the initial synthesis method employed. Single-phase rhombohedral samples exhibit the best thermoelectric properties but can only be obtained after an annealing step at 600 °C during initial cooling from the melt. Under faster cooling conditions, the samples obtained are inhomogeneous, containing multiple rhombohedral phases with a range of lattice parameters and exhibiting inferior thermoelectric properties. We also find that when the room-temperature rhombohedral phase is heated, an intermediate trigonal structure containing ordered cation vacancy layers is formed at ∼200 °C, driven by the spontaneous precipitation of argyrodite-type Ag₈GeTe₆ which alters the stoichiometry of the TAGS-85 matrix. The rhombohedral and trigonal phases of TAGS-85 coexist up to 380 °C, above which a single cubic phase is obtained and the Ag₈GeTe₆ precipitates redissolve into the matrix. On subsequent cooling a mixture of rhombohedral, trigonal, and Ag₈GeTe₆ phases is again obtained. Initially single-phase samples exhibit thermoelectric power factors of up to 0.0035 W m^-1 K^-2 at 500 °C, a value that is maintained on subsequent thermal cycling and which represents the highest power factor yet reported for undoped TAGS-85. Therefore, control over the structural homogeneity of TAGS-85 as demonstrated here is essential in order to optimize the thermoelectric performance.

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The structural, optical, and electrical transformations induced by hydrogen absorption and/or desorption in Mg-Ti thin films prepared by co-sputtering of Mg and Ti are investigated. Highly reflective in the metallic state, the films become highly absorbing upon H absorption. The reflector-to-absorber transition is fast, robust, and reversible over many cycles. Such a highly absorbing state hints at the coexistence of a metallic and a semiconducting phase. It is, however, not simply a composite material consisting of independent Mg H2 and Ti H2 grains. By continuously monitoring the structure during H uptake, we obtain data that are compatible with a coherent structure. The average structure resembles rutile Mg H2 at high Mg content and is fluorite otherwise. Of crucial importance in preserving the reversibility and the coherence of the system upon hydrogen cycling is the accidental equality of the molar volume of Mg and Ti H2. The present results point toward a rich and unexpected chemistry of Mg-Ti-H compounds.

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Hydrogen absorption by a thin Mg₂Ni film capped with Pd results in the nucleation of the Mg₂NiH₄ phase at the film/substrate interface. On further hydrogenation, a self-organized two-layer system consisting of a Mg₂NiH_0.3/Mg₂NiH₄ bottom-layer and a Mg₂NiH_0.3 top-layer is formed. This leads to an intermediate optical black state in Mg₂Ni thin films, which transforms from metallic/reflective to semiconducting/transparent upon hydrogenation. This hydrogen absorption behavior is completely unexpected, since the hydrogen enters the film through the Pd-capped film surface. To explain the preferential nucleation of Mg₂NiH₄ at the substrate/film interface, we determine the chemical homogeneity of these thin films by RBS and SIMS. Furthermore by STM, TEM and SEM, we analyze the microstructure. We find that up to a film thickness of 50 nm, the film consists of small grains and clusters of small grains. On further growth, a columnar structure develops. We propose that the nucleation barrier for the formation of the Mg₂NiH₄ phase is smaller for the small loosely packed grains at the interface, while the columnar grain boundaries promote the hydrogen diffusion to the substrate.

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Mg₂NiH₄ thin films have been prepared by activated reactive evaporation in a molecular beam epitaxy system equipped with an atomic hydrogen source. The optical reflection spectra and the resistivity of the films are measured in situ during deposition. In situ grown Mg₂NiH ₄ appears to be stable in vacuum due to the fact that the dehydrogenation of the Mg₂NiH₄ phase is kinetically blocked. Hydrogen desorption only takes place when a Pd cap layer is added. The optical band gap of the in situ deposited Mg₂NiH₄ hydride, 1.75 eV, is in good agreement with that of Mg₂NiH₄ which has been formed ex situ by hydrogenation of metallic Pd capped Mg₂Ni films. The microstructure of these in situ grown films is characterized by a homogeneous layer with very small grain sizes. This microstructure suppresses the preferred hydride nucleation at the film/substrate interface which was found in as-grown Mg₂Ni thin films that are hydrogenated after deposition.

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Although vortex pinning in laser-ablated YBa2Cu3O7-δ films on (100) SrTiO3 is dominated by threading dislocations (Dam B et al (1999) Nature 399 439), many other natural pinning sites are present. To identify the contribution from twin planes, surface corrugations and point defects, we manipulate the relative densities of all defects by post-annealing films with various as-grown dislocation densities, ndisl. While a universal magnetic field B dependence of the transport current density js (B, T) is observed (independently of ndisl, temperature T and the annealing treatment), the defect structure changes considerably. Correlating the microstructure to js (B, T), it becomes clear that surface roughness, twins and point defects are not important at low magnetic fields compared to linear defect pinning. Transmission electron microscopy indicates that threading dislocations are not part of grain boundaries nor are they related to the twin domain structure. We conclude that js (B, T) is essentially determined by pinning along threading dislocations, naturally induced during the growth process. Even in high magnetic fields, where the vortex density outnumbers ndisl, it appears that linear defects stabilize the vortex lattice by means of the vortex-vortex interaction.@en

The detailed mechanisms of the structural phase transformations that occur in epitaxial Y-hydride switchable mirrors are revealed with high resolution transmission electron microscopy (both cross sectional and plan view). The triangular ridge network that develops in Y prior to the α-β transformation is a result of 101̄2 deformation twinning. The basal plane that is originally parallel to the film/substrate interface is rotated by twinning over 5.6° and transformed into a prismatic plane and similarly the prismatic plane is transformed into a basal plane giving a final crystal reorientation for the ridge of 95.6°. After transformation to β, nearly vertical Σ3111 twin boundaries arise in the ridges. In contrast, horizontal twin boundaries develop in the β domains to prevent macroscopic shape changes. Inbetween the two twin variants within the domains, Shockley partial dislocations are persistently present, which enable efficient reversible β-γ switching of the mirror.

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