Search Results (106)

Fabrication aspects of PdO thin films and coatings are reviewed here. The work provides and organizes the up-to-date information on the methods to obtain the films. In recent years, the interest in Pd oxide for different applications has increased. Since Pd can be converted into PdO, it is instructive to pay attention to the preparation of the pure and the alloyed Pd films, heterostructures, and nanoparticles synthesized on different substrates. The development of PdO films is presented from the early reports on coatings’ formation by oxidation of Pd foils and wires to present technologies. Modern synthesis/growth routes are gathered into chemical and physical categories. Chemical methods include hydrothermal, electrochemical, electroless deposition, and coating methods, such as impregnation, precipitation, screen printing, ink jet printing, spin or dip coating, chemical vapor deposition (CVD), and atomic layer deposition (ALD), while the physical ones include sputtering and cathodic arc deposition, laser ablation, ion or electron beam-induced deposition, evaporation, and supersonic cluster beam deposition. Analysis of publications indicates that many as-deposited Pd or Pd-oxide films are granular, with a high variety of morphologies and properties targeting very different applications, and they are grown on different substrates. We note that a comparative assessment of the challenges and quality among different films for a specific application is generally missing and, in some cases, it is difficult to make a distinction between a film and a randomly oriented, powder-like (granular), thin compact material. Textured or epitaxial films of Pd or PdO are rare and, if orientation is observed, in most cases, it is obtained accidentally. Some practical details and challenges of Pd oxidation toward PdO and some specific issues concerning application of films are also presented. Full article

In metal additive manufacturing, reusing collected powder from previous builds is a standard practice driven by the substantial cost of metal powder. This approach not only reduces material expenses but also contributes to sustainability by minimizing waste. Despite its benefits, powder reuse introduces challenges related to maintaining the structural integrity of the components, making it a critical area of ongoing research and innovation. The reuse process can significantly alter powder characteristics, including flowability, size distribution, and chemical composition, subsequently affecting the microstructures and mechanical properties of the final components. Achieving repeatable and consistent printing outcomes requires powder particles to maintain specific and consistent physical and chemical properties. Variations in powder characteristics can lead to inconsistencies in the microstructural features of printed components and the formation of process-induced defects, compromising the quality and reliability of the final products. Thus, optimizing the powder recovery and reuse methodology is essential to ensure that cost reduction and sustainability benefits do not compromise product quality and reliability. This study investigated the impact of powder reuse and particle size distribution on the microstructural and mechanical properties of Ti-6Al-4V specimens fabricated using a laser beam directed energy deposition technique. Detailed evaluations were conducted on reused powders with two different size distributions, which were compared with their virgin counterparts. Microstructural features and process-induced defects were examined using scanning electron microscopy and X-ray computed tomography. The findings reveal significant alterations in the elemental composition of reused powder, with distinct trends observed for small and large particles. Additionally, powder reuse substantially influenced the formation of process-induced defects and, consequently, the fatigue performance of the components. Full article

The concept of measurement traceability is crucial for ensuring the data reliability and the comparability of measurement results provided by different instruments and operators. In the field of nanoparticle metrology, determining the size of nanoparticles using electron microscopy-based techniques remains a real challenge. In laboratory settings, the establishment of traceability regarding the instrument calibration procedures, the assessment of uncertainties associated with instruments/operators/samples/environments, as well as the complexities related to electron–sample interactions, are often neglected. In this article, we describe the calibration procedure set up at the LNE (Laboratoire National de métrologie et d’Essais) and propose an evaluation method for determining the uncertainties in measuring nanoparticle size by SEM (Scanning Electron Microscopy). This study investigates the impact of the energy of the primary electrons (PEs) generated by the electron beam and accelerating voltage on the reliability of size measurements. The convolution between the signals coming from a nanoparticle and the substrate on which the particle is deposited induces edge effects that can have a negative impact on the measurement results. Finally, a diagram describing the various stages involved in establishing traceability for SEM measurements of nanoparticle size is proposed to facilitate the work of future operators. Full article

The additive manufacturing (AM) of functional copper (Cu) parts is a major goal for many industries, from aerospace to automotive to electronics, because Cu has a high thermal and electrical conductivity as well as being ~10× cheaper than silver. Previous studies on AM of Cu have concentrated mainly on high-energy manufacturing processes such as Laser Powder Bed Fusion, Electron Beam Melting, and Binder Jetting. These processes all require high-temperature heat treatment in an oxygen-free environment. This paper shows an AM route to multi-layered microparts from novel nanoparticle (NP) Cu feedstocks, performed in an air environment, employing a low-power (<10 W) laser sintering process. Cu NP ink was deposited using two mechanisms, inkjet printing, and bar coating, followed by low-power laser exposure to induce particle consolidation. Initial parts were manufactured to a height of approximately 100 µm, which was achieved by multi-layer printing of 15 (bar-coated) to 300 (inkjetted) layers. There was no evidence of oxidised copper in the sintered material, but they were found to be low-density, porous structures. Nonetheless, electrical resistivity of ~28 × 10⁻⁸ Ω m was achieved. Overall, the aim of this study is to offer foundational knowledge for upscaling the process to additively manufacture Cu 3D parts of significant size via sequential nanometal ink deposition and low-power laser processing. Full article

The exploration initiated by the discovery of the topological insulator (Bi_xSb_1−x)₂Te₃ has extended to unlock the potential of quantum anomalous Hall effects (QAHEs), marking a revolutionary era for topological quantum devices, low-power electronics, and spintronic applications. In this study, we present the epitaxial growth of Cr-doped (Bi_0.4Sb_0.6)₂Te₃ (Cr:BST) thin films via molecular beam epitaxy, incorporating various Cr doping concentrations with varying Cr/Sb ratios (0.025, 0.05, 0.075, and 0.1). High-quality crystalline of the Cr:BST thin films deposited on a c-plane sapphire substrate has been rigorously confirmed through reflection high-energy electron diffraction (RHEED), X-ray diffraction (XRD), and high-resolution transmission electron microscopy (HRTEM) analyses. The existence of a Cr dopant has been identified with a reduction in the lattice parameter of BST from 30.53 ± 0.05 to 30.06 ± 0.04 Å confirmed by X-ray diffraction, and the valence state of Cr verified by X-ray photoemission (XPS) at binding energies of ~573.1 and ~583.5 eV. Additionally, the influence of Cr doping on lattice vibration was qualitatively examined by Raman spectroscopy, revealing a blue shift in peaks with increased Cr concentration. Surface characteristics, crucial for the functionality of topological insulators, were explored via Atomic Force Microscopy (AFM), illustrating a sevenfold reduction in surface roughness as the Cr concentration increased from 0 to 0.1. The ferromagnetic properties of Cr:BST were examined by a superconducting quantum interference device (SQUID) with a magnetic field applied in out-of-plane and in-plane directions. The Cr:BST samples exhibited a Curie temperature (T_c) above 50 K, accompanied by increased magnetization and coercivity with increasing Cr doping levels. The introduction of the Cr dopant induces a transition from n-type ((Bi_0.4Sb_0.6)₂Te₃) to p-type (Cr:(Bi_0.4Sb_0.6)₂Te₃) carriers, demonstrating a remarkable suppression of carrier density up to one order of magnitude, concurrently enhancing carrier mobility up to a factor of 5. This pivotal outcome is poised to significantly influence the development of QAHE studies and spintronic applications. Full article

Two-dimensional (2D) materials, characterized by their atomically thin nature and exceptional properties, hold significant promise for future nano-electronic applications. The precise control of carrier density in these 2D materials is essential for enhancing performance and enabling complex device functionalities. In this study, we present an electron-beam (e-beam) doping approach to achieve controllable carrier doping effects in graphene and MoS₂ field-effect transistors (FETs) by leveraging charge-trapping oxide dielectrics. By adding an atomic layer deposition (ALD)-grown Al₂O₃ dielectric layer on top of the SiO₂/Si substrate, we demonstrate that controllable and reversible carrier doping effects can be effectively induced in graphene and MoS₂ FETs through e-beam doping. This new device configuration establishes an oxide interface that enhances charge-trapping capabilities, enabling the effective induction of electron and hole doping beyond the SiO₂ breakdown limit using high-energy e-beam irradiation. Importantly, these high doping effects exhibit non-volatility and robust stability in both vacuum and air environments for graphene FET devices. This methodology enhances carrier modulation capabilities in 2D materials and holds great potential for advancing the development of scalable 2D nano-devices. Full article

Electron-induced fragmentation of the HFeCo₃(CO)₁₂ precursor allows direct-write fabrication of 3D nanostructures with metallic contents of up to >95 at %. While microstructure and composition determine the physical and functional properties of focused electron beam-induced deposits, they also provide fundamental insights into the decomposition process of precursors, as elaborated in this study based on EDX and TEM. The results provide solid information suggesting that different dominant fragmentation channels are active in single-spot growth processes for pillar formation. The use of the single source precursor provides a unique insight into high- and low-energy fragmentation channels being active in the same deposit formation process. Full article

Yttria-stabilized zirconia (YSZ), a thermal barrier coating material characterized by low thermal conductivity, is typically deposited via electron beam-physical vapor deposition. Notably, oxygen depletion occurs during this process, causing color changes in YSZ. Therefore, YSZ is speculated to undergo phase transformation during this process, which demands careful consideration owing to its effect on the life of thermal coatings. To study this phenomenon, bulk samples were prepared, subjected to vacuum heat treatment to induce oxygen depletion, and followed by oxidative heat treatment. Experimental results showed that the color of the samples changed to black after the vacuum heat treatment and to a lighter color after the oxidative heat treatment. In addition, X-ray diffraction and Raman analyses were performed. The monoclinic phase formation was confirmed during the vacuum heat treatment; however, it disappeared after the oxidation heat treatment. The coating obtained in a high vacuum atmosphere exhibited a black color and cubic phase, which changed to a bright color and tetragonal phase after the oxidation heat treatment. Full article

Magnonics is a rapidly developing domain of nanomagnetism, with application potential in information processing systems. Realisation of this potential and miniaturisation of magnonic circuits requires their extension into the third dimension. However, so far, magnonic conduits are largely limited to thin films and 2D structures. Here, we introduce 3D magnonic nanoconduits fabricated by the direct write technique of focused-electron-beam induced deposition (FEBID). We use Brillouin light scattering (BLS) spectroscopy to demonstrate significant qualitative differences in spatially resolved spin-wave resonances of 2D and 3D nanostructures, which originates from the geometrically induced non-uniformity of the internal magnetic field. This work demonstrates the capability of FEBID as an additive manufacturing technique to produce magnetic 3D nanoarchitectures and presents the first report of BLS spectroscopy characterisation of FEBID conduits. Full article

Nanomaterials with unique structures and functions have been widely used in the fields of microelectronics, biology, medicine, and aerospace, etc. With advantages of high resolution and multi functions (e.g., milling, deposition, and implantation), focused ion beam (FIB) technology has been widely developed due to urgent demands for the 3D fabrication of nanomaterials in recent years. In this paper, FIB technology is illustrated in detail, including ion optical systems, operating modes, and combining equipment with other systems. Together with the in situ and real-time monitoring of scanning electron microscopy (SEM) imaging, a FIB-SEM synchronization system achieved 3D controllable fabrication from conductive to semiconductive and insulative nanomaterials. The controllable FIB-SEM processing of conductive nanomaterials with a high precision is studied, especially for the FIB-induced deposition (FIBID) 3D nano-patterning and nano-origami. As for semiconductive nanomaterials, the realization of high resolution and controllability is focused on nano-origami and 3D milling with a high aspect ratio. The parameters of FIB-SEM and its working modes are analyzed and optimized to achieve the high aspect ratio fabrication and 3D reconstruction of insulative nanomaterials. Furthermore, the current challenges and future outlooks are prospected for the 3D controllable processing of flexible insulative materials with high resolution. Full article

The objective of this study is to explore and compare the mechanical response of AlCrSiN coatings deposited on two different substrates, namely, WC-Co and cBN. Nano-indentation was used to measure the hardness and elastic modulus of the coatings, and micro-indentation was used for observing the contact damage under Hertzian contact with monotonic and cyclic (fatigue) loads. Microscratch and contact damage tests were also used to evaluate the strength of adhesion between the AlCrSiN coatings and the two substrates under progressive and constant loads, respectively. The surface damages induced via different mechanical tests were observed using scanning electron microscopy (SEM). A focused ion beam (FIB) was used to produce a cross-section of the coating–substrate system in order to further detect the mode and extent of failure that was induced. The results show that the AlCrSiN coating deposited on the WC-Co substrate performed better in regard to adhesion strength and contact damage response than the same coating deposited on the cBN substrate; this is attributed to the lower plasticity of the cBN substrate as well as its less powerful adhesion to the coating. Full article

Laser Induced-Thermionic Vacuum Arc (LTVA) technology was used for depositing uniform intermetallic CoNi thin films of 100 nm thickness. LTVA is an original deposition method using a combination of the typical Thermionic Vacuum Arc (TVA) system and a laser beam provided by a QUANTEL Q-Smart 850 Nd:YAG compact Q-switched laser with a second harmonic module. The novelty is related to the simultaneous deposition of a bi-component metallic thin film using photonic processes of the laser over the plasma deposition, which improves the roughness but also triggers the composition of the deposited thin film. Structural analysis of the deposited thin films confirms the formation of face-centered cubic (fcc) as the main phase CoNi and hexagonal Co₃Ni as the minority phase, observed mainly using high-resolution transmission electron microscopy. The magneto-optical measurements suggest an isotropic distribution of the CoNi alloy thin films for the in-plan angular rotation. From the low coercive field of H_c = 40 Oe and a saturation field at 900 Oe, the CoNi thin films obtained by LTVA are considered semi-hard magnetic materials. Magnetic force microscopy reveals spherical magnetic nanoparticles with mean size of about 40–50 nm. The resistivity was estimated at $\rho$ = 34.16 μΩ cm, which is higher than the values for bulk Co and Ni. Full article

Gas-assisted focused electron-beam-induced deposition is a versatile tool for the direct writing of complex-shaped nanostructures with unprecedented shape fidelity and resolution. While the technique is well-established for various materials, the direct electron beam writing of silver is still in its infancy. Here, we examine and compare five different silver carboxylates, three perfluorinated: [Ag₂(µ-O₂CCF₃)₂], [Ag₂(µ-O₂CC₂F₅)₂], and [Ag₂(µ-O₂CC₃F₇)₂], and two containing branched substituents: [Ag₂(µ-O₂CCMe₂Et)₂] and [Ag₂(µ-O₂C^tBu)₂], as potential precursors for focused electron-beam-induced deposition. All of the compounds show high sensitivity to electron dissociation and efficient dissociation of Ag-O bonds. The as-deposited materials have silver contents from 42 at.% to above 70 at.% and are composed of silver nano-crystals with impurities of carbon and fluorine between them. Precursors with the shortest carbon-fluorine chain ligands yield the highest silver contents. In addition, the deposited silver content depends on the balance of electron-induced ligand co-deposition and ligand desorption. For all of the tested compounds, low electron flux was related to high silver content. Our findings demonstrate that silver carboxylates constitute a promising group of precursors for gas-assisted focused electron beam writing of high silver content materials. Full article

A systematic experimental study was performed to determine laser irradiation conditions for the large-area fabrication of highly regular laser-induced periodic surface structures (HR-LIPSS) on a 220 nm thick Mo film deposited on fused silica. The LIPSS were fabricated by scanning a linearly polarized, spatially Gaussian laser beam at 1030 nm wavelength and 1.4 ps pulse duration over the sample surface at 1 kHz repetition rate. Scanning electron microscope images of the produced structures were analyzed using the criterion of the dispersion of the LIPSS orientation angle (DLOA). Favorable conditions, in terms of laser fluence and beam scanning overlaps, were identified for achieving DLOA values <10${}^{\circ }$. To gain insight into the material behavior under these irradiation conditions, a theoretical analysis of the film heating was performed, and surface plasmon polariton excitation is discussed. A possible effect of the film dewetting from the dielectric substrate is deliberated. Full article

Magnetic force microscopy (MFM) is a powerful extension of atomic force microscopy (AFM), which mostly uses nano-probes with functional coatings for studying magnetic surface features. Although well established, additional layers inherently increase apex radii, which reduce lateral resolution and also contain the risk of delamination, rendering such nano-probes doubtful or even useless. To overcome these limitations, we now introduce the additive direct-write fabrication of magnetic nano-cones via focused electron beam-induced deposition (FEBID) using an HCo₃Fe(CO)₁₂ precursor. The study first identifies a proper 3D design, confines the most relevant process parameters by means of primary electron energy and beam currents, and evaluates post-growth procedures as well. That way, highly crystalline nano-tips with minimal surface contamination and apex radii in the sub-15 nm regime are fabricated and benchmarked against commercial products. The results not only reveal a very high performance during MFM operation but in particular demonstrate virtually loss-free behavior after almost 8 h of continuous operation, thanks to the all-metal character. Even after more than 12 months of storage in ambient conditions, no performance loss is observed, which underlines the high overall performance of the here-introduced FEBID-based Co₃Fe MFM nano-probes. Full article