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The focused ion beam (FIB) market is expected to grow from $820 million in 2019 to $1,185 million in 2024 and is already a well-known technology for electronics and semiconductor industry, materials science and it becomes more and more present in life sciences area.

International audience; The PELIICAEN (Platform for the Study of Ion Implantation Controlled and Analyzed at the Nanometric Scale) setup is a unique device, both for all of its in situ ultra-high vacuum equipment (focused ion beams (FIB) column, Secondary Electron Microscope (SEM), Atomic Force and Scanning Tunnelling Microscope (AFM/STM)), and for its nanostructuration performances on material. The setup has been recently equipped with its own electron cyclotron resonance ion sources, a new position-controlled platform using pneumatic vibration insulators and a fast pulsing device. Its performances were then deeply improved, providing access to a large choice of ions, an adjustable ion implantation depth up to few hundreds of nanometres, an image resolution down to 25 nm and an ion beam size on sample down to 100 nm. With all these equipment, the PELIICAEN setup is in the international foreground to perform and analyse ion implantation and surface modification.

Capillary-driven mass transport in solids is typically understood in terms of surface-diffusion limited kinetics, leading to conventional solid-state dewetting of thin films. However, another mass transport mechanism, so-called surface-attachment and detachment limited kinetics, is possible. It can shrink a solid film, preserving its original topology without breaking it in isolated islands, and leads to faster dynamics for smaller film curvature in contrast with the opposite behavior observed for surface-diffusion limited kinetics. In this work, we present a rimless dewetting regime for Si, which is ascribed to effective attachment-limited kinetics mediated by the coexistence of crystalline and amorphous Si phases. Phase-field numerical simulations quantitatively reproduce the experimental observations, assessing the main mass transport mechanism at play. The process can be exploited to obtain in a deterministic fashion monocrystalline islands (with 95% probability) pinned at ≈500 nm from a hole milled within closed patches.

Capillary-driven mass transport in solids is typically understood in terms of surface-diffusion limited kinetics, leading to conventional solid-state dewetting of thin films. However, another mass transport mechanism, so-called surface-attachment/detachment limited kinetics, is possible. It can shrink a solid film, preserving its original topology without breaking it in isolated islands, and leads to faster dynamics for smaller film curvature in contrast with the opposite behavior observed for surface-diffusion limited kinetics. In this work, we present a rimless dewetting regime for Si, which is ascribed to effective attachment-limited kinetics mediated by the coexistence of crystalline and amorphous Si phases. Phase-field numerical simulations quantitatively reproduce the experimental observations, assessing the main mass transport mechanism at play. The process can be exploited to obtain in a deterministic fashion monocrystalline islands (with $95%$ probability) pinned at $\ensuremath{\approx}500$ nm from a hole milled within closed patches.

International audience

International audience; Crystalline orientation maps are obtained in a Focused Ion Beam (FIB) microscope using the ion CHanneling ORientation Determination (iCHORD) method, which relies on the channeling phenomenon observed in ion-induced secondary electron images. The current paper focuses on the angular resolution that can be expected from such orientation maps, obtained using a revisited ion channeling model. A specific procedure was developed to evaluate the angular resolution, based on the distribution of orientation errors when evaluating controlled sample disorientation. The main advantage is that no external reference is required. An angular resolution of 1° is obtained on a nickel based sample using standard acquisition conditions. This value fulfills most of the needs in terms of microstructural characterization usually carried out by Electron Back Scattered Diffraction.

In order to check the manufacturing quality of electronic components using electron microscopy, the area of interest must be exposed. This requires the removal of a large quantity of matter without damaging the surrounding area. This step can be accomplished using ion milling but the processing can last a few hours. In order to accelerate the preparation of the samples, picosecond laser micromachining prior to Focused Ion Beam polishing is envisioned. Laser ablation allows the fast removal of matter but induces damages around the ablated area. Therefore the process has to be optimized in order to limit the size of both the heat affected zone and induced dislocation zone. For this purpose, cavities have been engraved in silicon and in electronic components, using a linearly polarized picosecond laser (∼50 ps) at three different wavelengths (343, 515 and 1030 nm). Results showed that the cross sectional shapes and the surface topologies can be tuned by the laser fluence and the number of pulses. Clear cross sections of bumps and cavity openings, exposing multilayer interfaces, are demonstrated. The silicon removal rates, tuned by the applied energy density, have been measured. Removal rates achieved at 200 kHz were typically hundred times higher than those achieved by ion milling and the best efficiency was obtained at 343 nm.

International audience; Dielectric Mie resonators have attracted a great deal of attention over the past few years thanks to their remarkable capabilities in manipulating light propagation at the nanoscale. However, the practical implementation of technological products is still elusive. One of the important limits is the absence of a high-performing material and a fabrication method that can be easily integrated into modern microelectronic devices at affordable costs. Here, we provide theoretical and experimental evidence of an alternative semiconductor material, SiGe alloys, for dielectric Mie resonator applications. As a material compatible with the processing requirements of the semiconductor industry, it possesses comparable optical properties to its conventional Si-based counterpart at visible frequencies in spite of its higher optical losses. These dielectric resonant 18 particles can be obtained over very large surfaces on arbitrary silica substrates via spontaneous solid state dewetting of ultrathin (

International audience; Thin film dewetting can be efficiently exploited for the implementation of functionalized surfaces over very large scales. Although the formation of sub-micrometer sized crystals via solid-state dewetting represents a viable method for the fabrication of quantum dots and optical meta-surfaces, there are several limitations related to the intrinsic features of dewetting in a crystalline medium. Disordered spatial organization, size, and shape fluctuations are relevant issues not properly addressed so far. This study reports on the deterministic nucleation and precise positioning of Si-and SiGe-based nanocrystals by templated solid-state dewetting of thin silicon films. The dewetting dynamics is guided by pattern size and shape taking full control over number, size, shape, and relative position of the particles (islands dimensions and relative distances are in the hundreds nm range and fluctuate approximate to 11% for the volumes and approximate to 5% for the positioning).

Nanopatterns of gold clusters on a large surface of oriented Si(111) substrates, from the galvanic displacement of gold salt (via the spontaneous reduction of AuCl4 -), are demonstrated in this work. The Si substrate is patterned by Focused Ion Beam (FIB) prior to being dipped in a gold solution. Here, we show that these patterns lead to successful control of the position and size of gold clusters. Sequential patterning reveals a powerful maskless alternative to surface preparation prior to Si nanowire growth.

The creation of nitrogen-vacancy centres in diamond is nowadays well controlled using nitrogen implantation and annealing. Although the high-resolution placement of NV centres has been demonstrated using either collimation through pierced AFM tips or masks with apertures made by electron beam lithography, a targeted implantation into pre-defined structures in diamond may not be achieved using these techniques. We show that a beam of nitrogen ions can be focused to approximately 100 nm using focused ion beam (FIB) technology. The nitrogen ion beam is produced using an electron cyclotron resonance (ECR) plasma source. Combined with a scanning electron microscope, the nitrogen-FIB offers new possibilities for the targeted creation of single defects in diamond. This maskless technology is suitable for example for the creation of optical centres in the cavities of photonic crystals or in diamond tips for scanning magnetometry. Finally, we further show that by changing the gas source from nitrogen to xenon, standard FIB milling capabilities are also available within the same tool.

International audience; Synthesizing Au 0.8 Si 0.2 nanocatalysts that are homogeneous in size and have controlled position is becoming a challenging and crucial prequisite for the fabrication of ordered semiconductor nanowires. In this study, Au 0.8 Si 0.2 nanocatalysts are synthesized via dewetting of Au layers on Si(111) during thermal annealing in an ultra-high vacuum. In the first part of the paper, the mechanism of homogeneous dewetting is analyzed as a function of the Au-deposited thickness ( h Au ). We distinguish three different dewetting regimes: (I) for a low thickness ( ##IMG## [http://ej.iop.org/images/0957-4484/26/50/505602/nano514960ieqn1.gif] \h_\\rmAu\\leqslant 0.4\\;\\mathrmnm\ ), a submonolyer coverage of Au is stabilized and there is no dewetting. (II) For an intermediate thickness ( ##IMG## [http://ej.iop.org/images/0957-4484/26/50/505602/nano514960ieqn2.gif] \0.4\\;\\mathrmnm\\lt h_\\mathrmAu\\leqslant 5\\;\\mathrmnm\ ), there is both dewetting and Au 0.8 Si 0.2 phase formation. The size and density of the Au 0.8 Si 0.2 clusters are directly related to h Au . When cooling down to room temperature, the clusters decompose and reject the Si at the Au/Si substrate interface. (III) For a large thickness ( ##IMG## [http://ej.iop.org/images/0957-4484/26/50/505602/nano514960ieqn3.gif] \h_\\rmAu\\gt 5\\;\\mathrmnm\ ), only dewetting takes place, without forming AuSi clusters. In this regime, the dewetting is kinetically controlled by the self-diffusion of Au (activation energy ∼0.43 eV) without evidence of an Si-alloying effect. As a practical consequence, when relying solely on the homogeneous dewetting of Au/Si(111) to form the Au 0.8 Si 0.2 catalysts (without a supply of Si atoms from vapor), regime II should be used to obtain good size and density control. In the second part of the paper, a process for ordering the catalysts using focused ion beam-(FIB) assisted dewetting (heterogeneous dewetting) is developed. We show that no matter what the FIB milling conditions and the Au nominal thickness are, dewetting is promoted by ion beam irradiation and is accompanied by the formation of Au 0.8 Si 0.2 droplets. The droplets preferentially form on the patterned areas, while in similar annealing conditions, they do not form on the unpatterned areas. This behavior is attributed to the larger Au-Si interdiffusion in the patterned areas, which results from the Si amorphization induced by the FIB. A systematic analysis of the position of the nanodroplets shows their preferential nucleation inside the patterns, while thicker platelets of almost pure Au are observed between the patterns. The evolutions of the size homogeneity and the occupancy rate of the patterns are quantified as a function of the FIB dose and annealing temperature. Nice arrays of perfectly ordered AuSi catalysts are obtained after optimizing the FIB and dewetting conditions.

International audience; The Andromede project is the center of a multi-disciplinary team which will build a new instrument for surface modification and analysis using the impact of probes from hydrogen to nano-particles (Au400+4) in the MeV range. For this new instrument a series of atomic, polyatomic, molecular and nano-particle ion beams will be delivered using two ion sources in tandem, a liquid metal ion source and an electron cyclotron resonance source. The delivered ion beams will be accelerated to high energy with a 4 MeV van de Graaff type accelerator. By using a suite of probes in the MeV energy range, ion beam analysis techniques, MeV atomic and cluster secondary ion mass spectrometry can all be performed in one location. A key feature of the instrument is its ability to produce an intense beam for injection into the accelerator. The commissioning of the two sources shows that intense beams from atomic ions to nano-particles can be delivered for subsequent acceleration. The calculations and measurements for the two sources are presented.

Selective growth and self-organization of silicon-germanium (SiGe) nanowires (NWs) on focused ion beam (FIB) patterned Si(111) substrates is reported. In its first step, the process involves the selective synthesis of Au catalysts in SiO2-free areas; its second step involves the preferential nucleation and growth of SiGe NWs on the catalysts. The selective synthesis process is based on a simple, room-temperature reduction of gold salts (Au3+Cl?/4 ) in aqueous solution, which provides well-organized Au catalysts. By optimizing the reduction process, we are able to generate a bidimensional regular array of Au catalysts with self-limited sizes positioned in SiO2 -free windows opened in a SiO /Si2 (111) substrate by FIB patterning. Such Au catalysts subsequently serve as preferential nucleation and growth sites of well-organized NWs. Furthermore, these NWs with tunable position and size exhibit the relevant features and bright luminescence that would find several applications in optoelectronic nanodevices.

Ni thin films deposited on (111) Al thick samples have been submitted to annealing treatment. The goal is to identify the phases formed in the early stage of mixing between Ni and Al. Combining complementary techniques such as x-ray absorption spectroscopy and x-ray photoelectron spectroscopy, we characterized two different systems depending on the temperature conditions. For a thermal treatment at 110 °C, a system formed of small AlNi3 clusters embedded in the Al matrix was identified. This was interpreted as due to the existence of a spontaneous Al/Ni interface mixed layer acting as a seed for the AlNi3 cluster formation. After annealing at 300 °C, the Al3Ni intermetallic compound was detected, in agreement with results in the literature.

International audience; Abstract In this work we study the influence of the major focused ion beam operating parameters: ion chemical species, beam current, lens voltage and ion dose on the ultimate nanopatterning resolution. We propose a two-step process based on first ion milling of a SiO2 sacrificial layer and second SiO2 chemical etching for the fabrication of nanopatterns with ultimate size/density and ad libitum shape. Examples of resulting patterns are presented.

International audience; We demonstrate that perfectly reproducible and homogeneous core-shell Si1−xGex/Ge nanowires can be produced by a two step nanofabrication process. The process makes use of a combination of Liquid Metal Alloy Ion Source–Focused Ion Beam (LMAIS-FIB) nanomilling and condensation. In a first step, we fabricate arrays of SiGe wires by LMAIS-FIB milling of fully relaxed Si1−xGex pseudo-substrates. The use of Ge2+ ions during this step avoids any metallic contamination of the nanowires. In a second step, we both reduce the diameter of the wires and form the core-shell configuration by oxido-reduction of the wires. Large arrays of core-shell nanowires with extended aspect ratio (length over diameter), small diameters and ultra-thin shell thickness are fabricated. Multilayer core-shell configurations with tunable arrangements could also be produced by repeated condensation cycles.

International audience; Design of monodisperse ultra-small nanocrystals (NCs) into large scale patterns with ad hoc features is demonstrated. The process makes use of solid state dewetting of a thin film templated through alloy liquid metal ion source focused ion beam (LMIS-FIB) nanopatterning. The solid state dewetting initiated at the edges of the patterns controllably creates the ordering of NCs with ad hoc placement and periodicity. The NC size is tuned by varying the nominal thickness of the film while their position results from the association of film retraction from the edges of the lay out and Rayleigh-like instability. The use of ultra-high resolution LMIS-FIB enables to produce monocrystalline NCs with size, periodicity, and placement tunable as well. It provides routes for the free design of nanostructures for generic applications in nanoelectronics.

Si3N4 amorphous thin layers prepared by sputtering have been implanted either with Cu or with Fe ions. X-ray absorption spectroscopy was performed at the Si K edge to characterise the electronic empty states of p character, the structural state of the initial layers and the modifications around Si induced by implantation and a post-annealing treatment. We show that the energy deposition process mainly leads to a reorganisation of the second coordination shell around Si, i.e. concerns the Si-Si bonds.

AlN bulk ceramic has been implanted with energetic Co ions. In order to accurately characterise the atomic surrounding of the implanted ions, X-ray absorption measurements were carried out at 80 K in the fluorescence mode at the Co K edge in the as-implanted and annealed states. Simulation of the EXAFS oscillations allowed us to identify a first stage where Co is inserted in the AlN matrix followed by a second stage where Co precipitates form., Facultad de Ciencias Exactas, Instituto de Física La Plata

Pressure is a unique tool to tune the interplay between structural, electronic and magnetic interactions. It leads to remarkable properties of materials such as recent temperature records in superconductivity. Advanced magnetic measurements under very high pressure in the Diamond Anvil Cell (DAC) use synchrotron approaches but these are lacking a formal link to the macroscopic magnetic properties. We report an alternative method consisting in optical magnetometry based on nitrogen-vacancy (NV) centers created at the surface of a diamond anvil. We illustrate the method by two measurements realized at room and low temperature respectively: the pressure evolution of the magnetization of an iron bead up to 30 GPa showing the iron ferromagnetic collapse and the detection of the superconducting transition of MgB2 at 7 GPa., 15 pages, 4 figures